CN109355051B - A kind of aqueous joint trimming agent and preparation method thereof - Google Patents
A kind of aqueous joint trimming agent and preparation method thereof Download PDFInfo
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- CN109355051B CN109355051B CN201811333182.9A CN201811333182A CN109355051B CN 109355051 B CN109355051 B CN 109355051B CN 201811333182 A CN201811333182 A CN 201811333182A CN 109355051 B CN109355051 B CN 109355051B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention provides a kind of aqueous joint trimming agent, is made of component A and B component by the mass ratio of 1:1；The component A includes that following mass fraction prepares raw material: 78~92 parts of bisphenol A type epoxy resin, 8~22 parts of polyether monoamine, 2~8 parts of hydrophilic fumed silica；The B component includes that following mass fraction prepares raw material: 40~55 parts of isophorone diamine, 20~25 parts of bisphenol A type epoxy resin, 18~28 parts of benzyl alcohol, 6~12 parts of emulsifier, 4~8 parts of hydrophilic fumed silica.The invention belongs to environment-friendly materials technical fields, aqueous joint trimming agent formula provided by the invention is simple, and durability is good, has the erasable function of water, conducive to the cleaning treatment after construction, it is nontoxic after solidification, VOC free discharge, surface hardness height, resistance to marring is strong, and there is excellent flexibility and cementability, phenomena such as being not in dusting and is mouldy, aesthetics is good.
Description
Technical field
The invention belongs to environment-friendly materials technical fields more particularly to a kind of aqueous joint trimming agent and preparation method thereof.
Background technique
The materials such as ceramic tile, mosaic are widely used in building decoration area, need when laying each block of material it
Between and corner etc. there are gaps.Traditional gap filler mainly uses white cement etc., has construction simple, lower-cost excellent
Point, but durability is poor, is easy occur phenomena such as dusting, blackening over time, and there is environmental protection and health etc.
Deficiency, overall performance is poor.
With the development of technology, oiliness two-component joint trimming agent is gradually instead of white cement for filling.Oiliness two-component beauty
Seam agent is the polymer not soluble in water that epoxy resin is formed by the amine curing agent containing active hydrogen by open loop crosslinking curing,
Have many advantages, such as that bonding force is good, intensity is high, surface is smooth, but presence is not environmentally friendly enough, is easy to appear cracking etc. after solidifying
Problem does not have the erasable function of water, is unfavorable for subsequent cleaning treatment.Existing commercially available ceramic tile epoxy joint trimming agent, it tends to be difficult to
Take into account cementability, durability and environmental-protecting performance.
107353857 A of Chinese patent application CN discloses a kind of epoxy joint trimming agent composition, including component A and B group
Point, wherein component A includes the raw materials such as epoxy resin, toughener, diluent, dispersing agent and filler, and B component includes polyetheramine, rouge
Cyclammonium, triethanolamine, diluent and filler have good bonding, anti-cracking performance, but ask there are constituent is more complex
Topic, and the epoxy joint trimming agent composition provided does not have the erasable function of water.
With environmental consciousness and improvement of living standard, more stringent requirements are proposed to joint trimming agent by consumer.Therefore, it mentions
It is of great significance for a kind of aqueous joint trimming agent for taking into account cementability, durability and environmental-protecting performance.
Summary of the invention
To solve problems of the prior art, inventor is by introducing specific knot in oiliness bisphenol A type epoxy resin
The Hydrophilicrto polyether monoamine of structure, then react to obtain water-soluble epoxy resin through high temperature polymerization, which can be added clear water and water is made
Property epoxy emulsion, more environment protection significance；Manufactured water-soluble epoxy resin, through hydrophily amine curing agent open loop cross-linking reaction,
The water-base epoxy polymer with high glaze is formed, which has the smooth glaze of oiliness epoxy, high intensity, high bonding
The characteristics of power, high tenacity, avoids ceramic tile and mosaic etc. and warps because of the internal stress of the generation of expanding with heat and contract with cold of Changes in weather
The problem of loosening；Simultaneously as the glaze that surface is formed makes mould be difficult to adsorb, and it is easy to clean, and color is transparent, nontoxic nothing
Evil.
The purpose of the present invention will be further described in detail below reflect and description.
The present invention provides a kind of aqueous joint trimming agent, is made of component A and B component by the mass ratio of 1:1；The component A packet
Include following mass fraction prepares raw material: 78~92 parts of bisphenol A type epoxy resin, 8~22 parts of polyether monoamine, hydrophily gas phase two
2~8 parts of silica；The B component includes that following mass fraction prepares raw material: 40~55 parts of isophorone diamine, bisphenol A-type
20~25 parts of epoxy resin, 18~28 parts of benzyl alcohol, 6~12 parts of emulsifier, 4~8 parts of hydrophilic fumed silica；It is described poly-
Ether monoamine is purchased from Huntsman Corporation, the U.S., product number M-2070.
It is the polymerization containing more than two epoxy groups in molecule that raw materials bisphenol A type epoxy resin is prepared selected by the present invention
Object has many advantages, such as that bonding force is preferable, shrinking percentage is low and chemicals-resistant；Its structure of polyether monoamine M-2070 selected by the present invention
Formula is CH3O(CH2CH2O)6-[CH2CH(R)O]n-CH2CH(CH3)-NH2, R is H or CH in formula3, there is stronger hydrophily,
Hydrophilic polyether segment and hydrophobic epoxy segment together constitute typical surfactant structure, after grafting to reach
To the purpose of aqueous epoxy resins；Selected hydrophilic fumed silica can give glue good resist sagging, vertically to apply
The offer of work point is good can application property；Selected curing agent isophorone diamine is the additive of Curing Waterborne Epoxy Resin, tool
There is the active hydrogen of high level, makes aqueous epoxy resins at normal temperature can solidified forming；Selected benzyl alcohol is as promotor, auxiliary
Curing agent fast solidification water epoxy resin；Selected emulsifier is the stearate of special hydrophilic functional group, is non-ionic
Emulsifier can increase the hydrophily of curing agent, the mesh quickly to mix both when reaching aqueous epoxy resins and curing agent mixing
's.
The above-mentioned combination and its dosage for preparing raw material, is that inventor is determined by a large number of experiments.Water provided by the invention
Property joint trimming agent formula it is simple, durability is good, have the erasable function of water, conducive to the cleaning treatment after construction, nontoxic nothing after solidification
Evil, VOC free discharge, it is not in dusting that surface hardness is higher, and resistance to marring is strong, and has excellent flexibility and cementability
And phenomena such as mouldy, aesthetics are good.
Preferably, the component A includes that following mass fraction prepares raw material: 80~90 parts of bisphenol A type epoxy resin, poly-
10~20 parts of ether monoamine, 3~5 parts of hydrophilic fumed silica；The B component includes that following mass fraction prepares raw material:
40~50 parts of isophorone diamine, 20~25 parts of bisphenol A type epoxy resin, 20~25 parts of benzyl alcohol, 8~10 parts of emulsifier, parent
5~7 parts of aqueous fumed silica.
It is highly preferred that the component A includes that following mass fraction prepares raw material: 85 parts of bisphenol A type epoxy resin, polyethers
15 parts of monoamine, 4 parts of hydrophilic fumed silica；The B component includes that following mass fraction prepares raw material: isophorone two
40 parts of amine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, 10 parts of emulsifier, 5 parts of hydrophilic fumed silica.
Preferably, the molecular formula of the bisphenol A type epoxy resin is C21H23ClFNO2, viscosity at 25 DEG C is
13000cps, relative density 1.16, epoxide equivalent are 189~190.
Preferably, the molecular formula of the emulsifier is C19H38O2, structural formula isThe emulsifier that the present invention uses is nonionic emulsifier, in oiliness asphalt mixtures modified by epoxy resin
Rouge, oiliness curing agent play the role of critical mediator, both ends point during being changed into aqueous epoxy resins, waterborne curing agent
Other oleophylic with it is hydrophilic, can water oil mixing under good intermiscibility between the two be provided, so that mixture is formed uniform system.
Component A and B component are prepared in raw material, can also be comprising a small amount of dye component for being used to rich colors, will not be right
The performance of the aqueous joint trimming agent of the present invention has an impact.
In addition, including the following steps: the present invention also provides the preparation method of aqueous joint trimming agent
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 122~126 DEG C,
Polyether monoamine is added dropwise under the speed of agitator of 500~550r/min, after being added dropwise to complete, is warming up to 134~138 DEG C, in -0.08~-
It is stirred to react 3~4 hours under 0.1MPa, then venting vacuum and is cooled to 35~45 DEG C, puts into hydrophilic fumed silica,
After revolving speed is adjusted to 1400~1600r/min and is evacuated to -0.08~-0.1MPa stirring 18~25 minutes, stops stirring and simultaneously protect
After holding 8~15 minutes, venting vacuum, filtering and discharging is to get component A；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 ± 2 DEG C, under the speed of agitator of 500~550r/min
The intermediate blend is added dropwise, after being added dropwise to complete, puts into emulsifier, insulation reaction 2~2.5 hours, is cooled to after the reaction was completed
35~45 DEG C, putting into hydrophilic fumed silica, revolving speed be adjusted to 1400~1600r/min and is evacuated to -0.08~-
0.1MPa is stirred 18~25 minutes, and after stopping stirs and maintains 8~15 minutes, venting vacuum, filtering and discharging is to get B component；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
It is reacted by oiliness bisphenol A type epoxy resin with hydrophilic polyether monoamine and synthesizes to obtain hydrophilic matrix tablets, structural formula
It is as follows:
Wherein, R
For H or CH3, a is corresponding with the n in polyether monoamine M-2070 structural formula, and b=6, reaction temperature and speed of agitator are to hydrophilic epoxy
The preparation of resin has great influence, and the speed of agitator of 500~550r/min forms suitable shearing while realizing stirring
Effect.It vacuumizes, can remove the small molecule byproduct generated in impurity small molecule and reaction in polyether monoamine presence, reach
To the effect of taste removal；Hydrophilic fumed silica is physics addition, is vertical its purpose is that giving glue good resist sagging
Straight construction point offer is good can application property.
Preferably, in the step 1), revolving speed is adjusted to 1500r/min；In the step 2), revolving speed is adjusted to 1500r/min.
Compared with prior art, the beneficial effect comprise that the present invention is with oiliness bisphenol A type epoxy resin and hydrophilic
Property polyether monoamine etc. to prepare raw material through high temperature polymerization reaction etc. obtain the aqueous joint trimming agent of high glaze.It is provided by the invention aqueous
Joint trimming agent formula is simple, and durability is good, has the erasable function of water, conducive to the cleaning treatment after construction；It is nontoxic after solidification,
VOC free discharge, good environmental protection meet the related request of GB 18583-2008；Smooth glaze can be formed, surface hardness is higher,
Resistance to marring is strong, and has excellent flexibility and cementability, phenomena such as being not in dusting and is mouldy, can avoid ceramic tile because of heat
Warp caused by swollen shrinkage physical phenomenon, fragmentation the problems such as, extend ceramic tile service life；Aesthetics is good, beautiful lasting, does not lose
Light.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
It is related to prepare the conventional raw material or commercial product that raw material is this field, polyethers list in the embodiment of the present invention
Amine is purchased from Huntsman Corporation, the U.S., product number M-2070.
The aqueous joint trimming agent of embodiment one
Aqueous joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes following mass fraction
Prepare raw material: 90 parts of bisphenol A type epoxy resin, 10 parts of polyether monoamine, 5 parts of hydrophilic fumed silica；The B component packet
Include following mass fraction prepares raw material: 40 parts of isophorone diamine, 22 parts of bisphenol A type epoxy resin, 25 parts of benzyl alcohol, emulsification
8 parts of agent, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of aqueous joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 550r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is warming up to 135 DEG C, it is small to be stirred to react 3.5 under -0.1MPa
When, it then venting vacuum and is cooled to 40 DEG C, puts into hydrophilic fumed silica, revolving speed is adjusted to 1550r/min and vacuumizes
After twenty minutes to -0.1MPa stirring, stopping stirs and maintains -0.1MPa after ten minutes, and venting vacuum, filtering and discharging is to get A
Component；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 80 DEG C, under the speed of agitator of 550r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1550r/min and be evacuated to -0.1MPa stir 20 minutes, stop stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
The aqueous joint trimming agent of embodiment two
Aqueous joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes following mass fraction
Prepare raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component packet
Include following mass fraction prepares raw material: 42 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsification
10 parts of agent, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of aqueous joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 520r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is warming up to 135 DEG C, it is small to be stirred to react 3.5 under -0.1MPa
When, it then venting vacuum and is cooled to 40 DEG C, puts into hydrophilic fumed silica, revolving speed is adjusted to 1500r/min and vacuumizes
After twenty minutes to -0.1MPa stirring, stopping stirs and maintains -0.1MPa after ten minutes, and venting vacuum, filtering and discharging is to get A
Component；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 520r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1500r/min and be evacuated to -0.1MPa stir 20 minutes, stopping stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
The aqueous joint trimming agent of embodiment three
Aqueous joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes following mass fraction
Prepare raw material: 80 parts of bisphenol A type epoxy resin, 20 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component packet
Include following mass fraction prepares raw material: 45 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 20 parts of benzyl alcohol, emulsification
9 parts of agent, 6 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of aqueous joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 500r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is warming up to 135 DEG C, is stirred under -0.08~-0.1MPa negative pressure
Then reaction 3.5 hours venting vacuum and is cooled to 40 DEG C, puts into hydrophilic fumed silica, revolving speed is adjusted to 1400r/min
And be evacuated to -0.1MPa stirring after twenty minutes, stop stirring and maintain -0.1MPa after ten minutes, venting vacuum filters out
Material is to get component A；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 500r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1400r/min and be evacuated to -0.1MPa stir 20 minutes, stopping stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
Comparative example 1
Joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes the preparation of following mass fraction
Raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component includes as follows
Mass fraction prepares raw material: 42 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsifier 10
Part, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-600；；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 520r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is warming up to 135 DEG C, is stirred to react under -0.08~-0.1MPa
It 3.5 hours, then venting vacuum and is cooled to 40 DEG C, puts into hydrophilic fumed silica, revolving speed is adjusted to 1500r/min and takes out
Vacuum stirs after twenty minutes to -0.1MPa, and stopping stirs and maintains -0.1MPa after ten minutes, venting vacuum, filtering and discharging, i.e.,
Obtain component A；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 520r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1500r/min and be evacuated to -0.1MPa stir 20 minutes, stop stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
Comparative example 1 is from the difference of embodiment two: polyether monoamine is different.
Comparative example 2
Joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes the system of following mass fraction
Standby raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component includes such as
Lower mass fraction prepares raw material: 42 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsifier 10
Part, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The emulsifier is commercially available conventional emulsifier odium stearate.
The preparation method of joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 520r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is warming up to 135 DEG C, is stirred to react under -0.08~-0.1MPa
It 3.5 hours, then venting vacuum and is cooled to 40 DEG C, puts into hydrophilic fumed silica, revolving speed is adjusted to 1500r/min and takes out
Vacuum stirs after twenty minutes to -0.1MPa, and stopping stirs and maintains -0.1MPa after ten minutes, venting vacuum, filtering and discharging, i.e.,
Obtain component A；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 520r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1500r/min and be evacuated to -0.1MPa stir 20 minutes, stopping stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
Comparative example 2 is from the difference of embodiment two: emulsifier is different.
Comparative example 3
Joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes the system of following mass fraction
Standby raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component includes such as
Lower mass fraction prepares raw material: 42 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsifier 10
Part, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C,
Polyether monoamine is added dropwise under the speed of agitator of 1500r/min, after being added dropwise to complete, is warming up to 135 DEG C, is stirred under -0.08~-0.1MPa
Reaction 3.5 hours is mixed, then venting vacuum and 40 DEG C is cooled to, puts into hydrophilic fumed silica, revolving speed is adjusted to 1500r/
Min is simultaneously evacuated to -0.1MPa stirring after twenty minutes, and stopping stirs and maintains -0.1MPa after ten minutes, venting vacuum, filtering
Discharging is to get component A；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 520r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1500r/min and be evacuated to -0.1MPa stir 20 minutes, stopping stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
Comparative example 3 is with the difference of embodiment two: revolving speed when bisphenol A type epoxy resin is reacted with polyether monoamine is not
Together.
Comparative example 4
Joint trimming agent is made of component A and B component by the mass ratio of 1:1；The component A includes the system of following mass fraction
Standby raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component includes such as
Lower mass fraction prepares raw material: 42 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsifier 10
Part, 5 parts of hydrophilic fumed silica.
The polyether monoamine is M-2070；The molecular formula of the emulsifier is C19H38O2, structural formula is
The preparation method of aqueous joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 125 DEG C, 520r/
Polyether monoamine is added dropwise under the speed of agitator of min, after being added dropwise to complete, is stirred to react 3.5 hours under -0.08~-0.1MPa, then
Venting vacuum is simultaneously cooled to 40 DEG C, puts into hydrophilic fumed silica, and revolving speed is adjusted to 1500r/min and to be evacuated to-
0.1MPa is stirred after twenty minutes, and stopping stirs and maintains -0.1MPa after ten minutes, and venting vacuum, filtering and discharging is to get A group
Part；
2) make B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank obtain it is intermediate mixed
Object is closed, weighs isophorone diamine in the second reaction vessel, is warming up to 78 DEG C, under the speed of agitator of 520r/min described in dropwise addition
Intermediate blend after being added dropwise to complete, puts into emulsifier, insulation reaction 2 hours, is cooled to 40 DEG C after the reaction was completed, puts into hydrophilic
Property fumed silica, revolving speed be adjusted to 1500r/min and be evacuated to -0.1MPa stir 20 minutes, stopping stir and maintain -
After ten minutes, venting vacuum, filtering and discharging is to get B component by 0.1MPa；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
Comparative example 4 is with the difference of embodiment two: temperature when bisphenol A type epoxy resin is reacted with polyether monoamine maintains
At 125 DEG C, it is not warming up to 135 DEG C.
Performance test example
Joint trimming agent made from above-described embodiment is tested for the property respectively, by above-described embodiment one to three and comparative example
Component A, the B component of 1-4 is not filled into the sebific duct of 1:1, loads onto epoxy glue mouth, is uniformly squeezed into ceramic tile using power-assisted glue rifle and is stitched
In, and with tooled joint bundle of spheres stitch in glue flatten, 25 DEG C of room temperature solidify 24 hours after carry out the tests of the indexs such as surface gloss, tie
Fruit is as shown in table 1.
The performance test results table of the different joint trimming agents of table 1
As known from Table 1, joint trimming agent provided by the invention has excellent water resistance, toughness and stability etc., and glossiness is high,
Has the erasable function of water, conducive to the cleaning treatment after construction.However, comparative example 1 can not be with oiliness due to polyether monoamine M-600
Bisphenol A type epoxy resin reaction synthesis obtains hydrophilic matrix tablets, leads to final products performance and significant difference of the present invention；It is right
Ratio 3 leads to the difference and shock resistance of shearing effect since revolving speed when bisphenol A type epoxy resin is reacted from polyether monoamine is different
Intensity is remarkably decreased, and leads to final products performance and significant difference of the present invention.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (6)
1. a kind of aqueous joint trimming agent, it is characterised in that: be made of component A and B component by the mass ratio of 1:1；The component A includes
Following mass fraction prepares raw material: 78 ~ 92 parts of bisphenol A type epoxy resin, 8 ~ 22 parts of polyether monoamine, hydrophily gas phase dioxy
2 ~ 8 parts of SiClx；The B component includes that following mass fraction prepares raw material: 40 ~ 55 parts of isophorone diamine, bisphenol-A type ring
20 ~ 25 parts of oxygen resin, 18 ~ 28 parts of benzyl alcohol, 6 ~ 12 parts of emulsifier, 4 ~ 8 parts of hydrophilic fumed silica；The polyethers list
Amine is purchased from Huntsman Corporation, the U.S., product number M-2070；
The molecular formula of the emulsifier is C19H38O2, structural formula is；
The preparation method of the aqueous joint trimming agent includes the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 122 ~ 126 DEG C, 500 ~
Polyether monoamine is added dropwise under the speed of agitator of 550r/min, after being added dropwise to complete, 134 ~ 138 DEG C are warming up to, under -0.08 ~ -0.1MPa
It is stirred to react 3 ~ 4 hours, then venting vacuum and is cooled to 35 ~ 45 DEG C, put into hydrophilic fumed silica, -0.08 ~ -
After being stirred 18 ~ 25 minutes under 0.1MPa with the revolving speed of 1400 ~ 1600r/min, after stopping stirs and maintains 8 ~ 15 minutes, venting is true
Sky, filtering and discharging is to get component A；
2) it makes B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank and obtain intermediate blend,
Isophorone diamine is weighed in the second reaction vessel, 78 ± 2 DEG C is warming up to, institute is added dropwise under the speed of agitator of 500 ~ 550r/min
Intermediate blend is stated, after being added dropwise to complete, emulsifier is put into, insulation reaction 2 ~ 2.5 hours, is cooled to 35 ~ 45 DEG C after the reaction was completed,
Hydrophilic fumed silica is put into, after being stirred 18 ~ 25 minutes under -0.08 ~ -0.1MPa with the revolving speed of 1400 ~ 1600r/min,
After stopping stirs and maintains 8 ~ 15 minutes, venting vacuum, filtering and discharging is to get B component；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
2. aqueous joint trimming agent according to claim 1, it is characterised in that: the component A includes the system of following mass fraction
Standby raw material: 80 ~ 90 parts of bisphenol A type epoxy resin, 10 ~ 20 parts of polyether monoamine, 3 ~ 5 parts of hydrophilic fumed silica；The B
Component includes that following mass fraction prepares raw material: 40 ~ 50 parts of isophorone diamine, 20 ~ 25 parts of bisphenol A type epoxy resin, benzene
20 ~ 25 parts of methanol, 8 ~ 10 parts of emulsifier, 5 ~ 7 parts of hydrophilic fumed silica.
3. aqueous joint trimming agent according to claim 2, it is characterised in that: the component A includes the system of following mass fraction
Standby raw material: 85 parts of bisphenol A type epoxy resin, 15 parts of polyether monoamine, 4 parts of hydrophilic fumed silica；The B component includes
Following mass fraction prepares raw material: 40 parts of isophorone diamine, 20 parts of bisphenol A type epoxy resin, 23 parts of benzyl alcohol, emulsification
10 parts of agent, 5 parts of hydrophilic fumed silica.
4. aqueous joint trimming agent according to any one of claim 1 to 3, it is characterised in that: the bisphenol A type epoxy resin
Molecular formula be C21H23ClFNO2, viscosity at 25 DEG C is 13000cps, and relative density 1.16, epoxide equivalent is 189 ~ 190.
5. the preparation method of aqueous joint trimming agent according to claim 1, characterized by the following steps:
1) it makes component A: weighing bisphenol A type epoxy resin and put into the first reaction vessel, be warming up to 122 ~ 126 DEG C, 500 ~
Polyether monoamine is added dropwise under the speed of agitator of 550r/min, after being added dropwise to complete, 134 ~ 138 DEG C are warming up to, under -0.08 ~ -0.1MPa
It is stirred to react 3 ~ 4 hours, then venting vacuum and is cooled to 35 ~ 45 DEG C, put into hydrophilic fumed silica, -0.08 ~ -
After being stirred 18 ~ 25 minutes under 0.1MPa with the revolving speed of 1400 ~ 1600r/min, after stopping stirs and maintains 8 ~ 15 minutes, venting is true
Sky, filtering and discharging is to get component A；
2) it makes B component: weighing bisphenol A type epoxy resin and benzyl alcohol, mix and be pumped into dropping tank and obtain intermediate blend,
Isophorone diamine is weighed in the second reaction vessel, 78 ± 2 DEG C is warming up to, institute is added dropwise under the speed of agitator of 500 ~ 550r/min
Intermediate blend is stated, after being added dropwise to complete, emulsifier is put into, insulation reaction 2 ~ 2.5 hours, is cooled to 35 ~ 45 DEG C after the reaction was completed,
Hydrophilic fumed silica is put into, after being stirred 18 ~ 25 minutes under -0.08 ~ -0.1MPa with the revolving speed of 1400 ~ 1600r/min,
After stopping stirs and maintains 8 ~ 15 minutes, venting vacuum, filtering and discharging is to get B component；
3) component A obtained and B component are mixed by the mass ratio of 1:1, obtains aqueous joint trimming agent.
6. the preparation method of aqueous joint trimming agent according to claim 5, it is characterised in that: in the step 1), revolving speed tune
To 1500r/min；In the step 2, revolving speed is adjusted to 1500r/min.
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| CN107353857A (en) * | 2017-06-20 | 2017-11-17 | 广州市白云化工实业有限公司 | Epoxy joint trimming agent composition and preparation method thereof |
| CN107691448A (en) * | 2017-10-18 | 2018-02-16 | 万华化学集团股份有限公司 | A kind of epoxy soybean oil base mould inhibitor and its preparation method and application, epoxy joint trimming agent |
| CN108018012A (en) * | 2017-12-05 | 2018-05-11 | 万华化学集团股份有限公司 | Joint trimming agent is with amine curing agent and preparation method thereof and the joint trimming agent composition epoxy resin including the curing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107353857A (en) * | 2017-06-20 | 2017-11-17 | 广州市白云化工实业有限公司 | Epoxy joint trimming agent composition and preparation method thereof |
| CN107691448A (en) * | 2017-10-18 | 2018-02-16 | 万华化学集团股份有限公司 | A kind of epoxy soybean oil base mould inhibitor and its preparation method and application, epoxy joint trimming agent |
| CN108018012A (en) * | 2017-12-05 | 2018-05-11 | 万华化学集团股份有限公司 | Joint trimming agent is with amine curing agent and preparation method thereof and the joint trimming agent composition epoxy resin including the curing agent |
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