CN108424521A - Water-based mono-component epoxy resin latex and preparation method thereof - Google Patents
Water-based mono-component epoxy resin latex and preparation method thereof Download PDFInfo
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Abstract
The invention discloses single-component epoxy lotions and preparation method thereof；This method first synthesizes the epoxy resin of unsaturated fatty acid modification；Simultaneously the hydrophilic segment that end carries carboxyl is prepared with cis-butenedioic anhydride and poly glycol monomethyl ether esterification, then the epoxy resin being modified with above-mentioned unsaturated fatty acid carries out esterification, hydrophilic segment is introduced on the side chain of epoxy resin, to prepare a kind of aqueous one-component epoxy emulsion.The paint film adhesion that the epoxy emulsion is formed is good, and hardness is high, and mechanical strength and good toughness, Corrosion Protection are excellent；And good storage stability and corrosion resistance are shown with coating prepared by this lotion.
Description
Technical field
The invention belongs to chemical technology fields, are related to a kind of matrix resin for the anticorrosive paint being mainly used for steel product, especially
It is related to a kind of preparation method with aqueous dispersible single-component epoxy lotion, while the invention further relates to water-base epoxy breasts
Liquid is applied in aqueous industrial anti-corrosion primer.
Background technology
Increasingly stringent with environmental protection, water paint gradually emerges.It compares for oil paint, water paint can be big
Amount reduces the use of organic solvent, to reduce the pollution to environment, reduces the potential hazard to operating personnel, and be convenient for work
Factory takes safety measures and transports, and as a kind of using water as the green environmental friendly coatings of solvent, has widely application prospect.
Currently used water-base resin includes aqueous epoxy resins, aqueous polyurethane, aqueous acrylic resin, water alcohol acid tree
Fat etc. and its modifier.For the substance that steel etc. easily corrodes, epoxy resin has excellent adhesive force, thermostabilization
The advantages that property, chemical-resistant, insulating properties agent mechanical strength, it is used as the preferred resin of steel protective coating for a long time.
The water-borne modification method of aqueous epoxy resins mainly has Mechanical Method, phase inversion, self-emulsification etc..Mechanical Method and opposite
Dispersion particle diameter prepared by robin is larger, and example is in irregular shape and wider distribution, and the stability of emulsion prepared is poor, especially
For the lotion of addition emulsifier, hardness of paint film, the performances such as water resistance are all poor.Method more common at present is self-emulsification,
By introducing hydrophilic radical on main chain, make the resin of preparation that there is water solubility, particle diameter distribution is more uniform, the paint film of preparation
It can be also more preferable.
However the epoxy resin prepared at present by self-emulsification, especially single component epoxy is often through being neutralized into
Salt or the raw material of complexity are prepared with technique, and for being neutralized into the epoxy emulsion of salt, it is easy to appear flash rustings in the construction process；
And the technological operation of higher cost of manufacture and complexity is then needed for another, so it is opposite to explore a kind of preparation process
Simply, the single-component water-based epoxy resin latex of the stronger preparation process of easy to operate versatility and better performances is necessary
Property.
Invention content
The present invention to be solved the above problems and is, provide it is a kind of it is simple for process, at low cost, with superperformance and environmentally friendly one
The single-component water-based epoxy resin latex and preparation method thereof of kind normal temperature self-drying.Its product advantage be using water as solvent, it is nontoxic
It is pollution-free, emulsion particle diameter is small, storage stability is good, paint film flat smooth, while again keep solvent epoxy varnish etching ground
The performances such as strong adhesive force, water-tolerant, chemicals-resistant and salt spray resistance be good.
One component room temperature according to the present invention is to use unsaturated fatty acid esterification by ring opening from dry aqueous epoxy emulsion
Modified epoxy, the hydrophilic segment with carboxyl then prepared with acid anhydrides and polyalkylene glycol monoalkyl ether be esterified anti-
It should be prepared.This method be chemical modification self-emulsification, the emulsion particle diameter of preparation is small, usually nm ranks, lotion it is steady
It sets, can keep not changing for 6 months.
It is to lean on unsaturated fatty acid that epoxy emulsion prepared by the present invention, which has room-temperature self crosslinking, self-crosslinking realization,
On carbon-carbon double bond autoxidation crosslinking realize.The self-crosslinking reaction of unsaturated fatty acid can accelerate the fast of lotion at room temperature
Dryness, the performances such as hardness, the richness of fast lifting paint film.
To achieve the above object, technical solution according to the present invention is：
The synthesis of first step unsaturated fatty acid modified epoxy
It is calculated with molal quantity, by epoxy group molal quantity and unsaturated fatty acid molal quantity according to 1-1.2:1 ratio is added to instead
It answers in device, stirring solvent is then added at homogeneous, the catalyst for the 0.01-0.05 that molal quantity is epoxy group molal quantity is added,
It is warming up to 120-150 DEG C of progress esterification, after reacting 3-5 hours, it is eventually that the acid value of detection architecture, which is the 5% or less of initial value,
The epoxy resin that room temperature unsaturated fatty acid is modified is made in point；
In the above scheme, the epoxy resin be by epoxychloropropane or methyl epichlorohydrin and bisphenol-A, Bisphenol F or
The polyglycidyl ether of the epoxyalkane merchant Chengwu of epoxy resin that bisphenol sulphone obtains, bisphenol-A, polypropylene glycol, 1,6- hexylene glycols,
The polyglycidyl ether of the polyalcohols such as trimethylolpropane, glycerine；Adipic acid, phthalic acid, dimer acid etc. are polycarboxylic poly-
Ethylene oxidic ester and poly epihydric alcohol amine etc..It is more preferably selected from the above-mentioned bisphenol-A of above-mentioned use or Bisphenol F and epoxychloropropane system
Epoxy resin made of the polycarboxylic acid of standby epoxy resin or adipic acid is modified.
In the above scheme, the unsaturated fatty acid is selected from oleic acid（Octadecenoic acid）, linoleic acid siritch（18
Two carbon enoic acids）, leukotrienes（18 carbon enoic acids）, siritch, tung oil, at least one of ricinoleic acid.
In the above scheme, the solvent to epoxy resin and unsaturated fatty acid and its reaction product have compared with
Good dissolving power and reactionlessness, and used solvent have preferably with the intersolubility of water.Selected solvent is selected from single
The glycol dinitrates such as glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, ethylene glycol monobutyl ether ethers and butyl ether
Class, ethylene glycol monobutyl ether；Propylene glycol monomethyl ether, propylene glycol monoethyl, glycol monobutyl ether, propylene glycol list isobutyl group
At least one of propylene-glycol monoalky lethers classes such as ether, propylene glycol list tertbutyl ether.
In above-mentioned scheme, the catalyst is butyl titanate, monomethyl tin oxide, triphenyl phosphorus and the tetrabutyl
At least one of ammonium bromide.
Second step prepares anhydride modified hydrophilic segment
In order to solve the water-wet behavior of modified epoxy, the hydrophilic chain with carboxyl is prepared by esterification in this step
Section, it with molar ratio is 1 that specific implementation method, which is by the poly glycol monomethyl ether of acid anhydrides and number-average molecular weight 400-2000,:1-
0.8 in catalyst（Weight is the 0.05-0.1 of poly glycol monomethyl ether）The lower progress esterification of effect is prepared.
Above-mentioned esterification reaction temperature is at 80-120 DEG C, and reaction time of esterification was at 2-5 hours.
In above-mentioned scheme, the acid anhydrides is selected from phthalic anhydride, acetic anhydride, maleic anhydride, succinic anhydride, phthalic acid
At least one of acid anhydride, o- benzoic acid acid anhydride.
In above-mentioned scheme, its number-average molecular weight of the poly glycol monomethyl ether is between 400-1000.
In above-mentioned scheme, the catalyst is selected from triethylamine, tri-n-butylamine, benzyldimethylamine, 2,4,2,4,6- tri- (two
Methylaminomethyl) phenol, the tertiary amines such as N methyl piperazine and its esters；2-methylimidazole, 2- phenylimidazoles, 2- undecyls
Imidazoles, 2-ethyl-4-methylimidazole；Tetraphenyl microcosmic salt, methyl tributyl microcosmic salt, methyl tricyanoethyl microcosmic salt, tetrabutyl phosphorus
At least one of salt.
Third walks the preparation of aqueous one-component epoxy emulsion；
The anhydride modified hydrophilic segment that the epoxy resin that unsaturated fatty acid prepared by the first step is modified is prepared with second step
Esterification is carried out under the effect of the catalyst, is eventually adding the epoxy emulsion that deionized water is prepared into aqueous one-component.
In the above scheme, specific experimentation be related to the epoxy resin for being modified 15-35 parts of unsaturated fatty acids with
15-35 parts of anhydride modified hydrophilic segments are in catalyst（0.05-0.1 parts）It is 80-120 DEG C in reaction temperature, reaction time control
After 2-5 hours, 40-60 DEG C is naturally cooled to, is kept under high-speed stirred state, it is 30- that deionized water, which is added, and prepares solid content
The single-component epoxy lotion of 70% solid content.
In above-mentioned scheme, the catalyst is selected from triethylamine, tri-n-butylamine, benzyldimethylamine, 2,4,2,4,6- tri- (two
Methylaminomethyl) phenol, the tertiary amines such as N methyl piperazine and its esters；2-methylimidazole, 2- phenylimidazoles, 2- undecyls
Imidazoles, 2-ethyl-4-methylimidazole；Tetraphenyl microcosmic salt, methyl tributyl microcosmic salt, methyl tricyanoethyl microcosmic salt, tetrabutyl phosphorus
At least one of salt.
In the above scheme, the first step and third step lotion preparation can carry out in same reaction kettle, therefore
It is easy to operate, it is energy saving.Gained aqueous one-component epoxy emulsion smell is small, and appearance is in faint yellow to yellow liquid, grain size point
Cloth is more uniform, and the storage stability of lotion is good, and storage in 6 months does not settle.
The one component room temperature from dry epoxy emulsion through spraying, brushing or dip-coating behind iron and steel material quality surface, in room temperature item
It is spontaneously dried seven days under part, gloss of film degree is high after film forming, and lacquer painting is smooth, and water-fast seven days without any whiting, salt spray resistance energy
Reach 168 hours or more.
Compared with the existing technology, beneficial effects of the present invention are as follows:
(1) single-component epoxy lotion prepared by the present invention, raw material sources are extensive, preparation process is easy, can be energy saving, improve
Efficiency.The single-component epoxy lotion of preparation farthest remains the excellent adhesion of epoxy resin, wearability, corrosion resistance
And the features such as mechanical strength.
(2) single-component epoxy lotion prepared by the present invention is packaged using single group, self-crosslinking can be solidified at room temperature
Film has easy to use compared to for more double-component aqueous epoxy, being not necessarily to when in use plus curing agent, and constructing operation is simple
Advantage.
(3) single-component epoxy lotion prepared by the present invention has hardness of paint film height, glossiness in room temperature from after doing seven days
The advantages that height, hardness of paint film is high, and corrosion-resistant and water resistance is good.
Description of the drawings
Fig. 1 is the flow chart that the present invention prepares aqueous one-component epoxy emulsion
Specific implementation mode
In order to better understand the present invention, it is to illustrate the phenol present invention with reference to specific example；
Embodiment 1
1. unsaturated fatty acid modified epoxy is prepared according to the raw material of following quality:By 190g epoxy resin E51 with
278g linoleic acids are added in reaction bulb, and 200g ethylene glycol monobutyl ethers are then added, and 1g triphenyl phosphorus, high-speed stirring is added
It mixes uniformly, is warming up to 130 DEG C or so, react 4 hours or so, then measure acid value, cool down when acid value is less than the 5% of initial value and stop
Only react；
2. the poly glycol monomethyl ether for the 400g that acetic anhydride 102g and molecular weight are 400 is added in reactor, it is added 1g's
Triethylamine, after stirring evenly, raising reaction temperature is to 100 DEG C, cooling discharge after reaction 3 hours；
3. taking 200g to take the mixture in 300g steps 1 to be added to instead with the reactant in step 1 reactant in step 2
It answers in device, the warming while stirring of 1g benzyldimethylamine, 2,4s is added to 90 DEG C, after reacting 4 hours, cools to 50 DEG C, deionization is added dropwise
Water 500g, after being added dropwise to complete, cooling discharge obtains the epoxy emulsion of one-component.
The lotion is weak yellow liquid, and 42% or so, viscosity 500-700mpa.s, comprehensive performance is seen below solid content
Table.
Embodiment 2
1. unsaturated fatty acid modified epoxy is prepared according to the raw material of following quality:By 190g epoxy resin E51 with
250g eleostearic acids are added in reaction bulb, and 200g dipropylene glycol methyl ethers are then added, and 1g triphenyl phosphorus is added, and high-speed stirred is equal
It is even, 120 DEG C or so are warming up to, is reacted 4 hours or so, then measures acid value, cooling stopping is anti-when acid value is less than the 5% of initial value
It answers；
2. the poly glycol monomethyl ether for the 600g that phthalic anhydride 148g and molecular weight are 600 is added in reactor, add
The triethylamine for entering 1g, after stirring evenly, raising reaction temperature is to 110 DEG C, cooling discharge after reaction 3 hours；
3. taking 350g to take the mixture in 300g steps 1 to be added to instead with the reactant in step 1 reactant in step 2
It answers in device, the warming while stirring of 1g triethylamines is added to 100 DEG C, after reacting 4 hours, cools to 50 DEG C, deionized water is added dropwise
350g, after being added dropwise to complete, cooling discharge obtains the epoxy emulsion of one-component.
The lotion is yellow liquid, and 55% or so, viscosity 800-1200mpa.s, comprehensive performance is seen below solid content
Table.
Embodiment 3
1. unsaturated fatty acid modified epoxy is prepared according to the raw material of following quality:By 250g epoxy resin E20 with
125g eleostearic acids are added in reaction bulb, and 200g dipropylenes are then added, and 1g triphenyl phosphorus is added, and high-speed stirred is equal
It is even, 120 DEG C or so are warming up to, is reacted 4 hours or so, then measures acid value, cooling stopping is anti-when acid value is less than the 5% of initial value
It answers；
2. the poly glycol monomethyl ether for the 600g that phthalic anhydride 148g and molecular weight are 600 is added in reactor, add
The triethylamine for entering 1g, after stirring evenly, raising reaction temperature is to 110 DEG C, cooling discharge after reaction 3 hours；
3. taking 350g to take the mixture in 550g steps 1 to be added to instead with the reactant in step 1 reactant in step 2
Answer in device, the warming while stirring of 1g benzyldimethylamine, 2,4s be added to 100 DEG C, after reaction 4 hours, cool to 60 DEG C, dropwise addition go from
Sub- water 1100g, after being added dropwise to complete, cooling discharge obtains the epoxy emulsion of one-component.
The lotion is yellow liquid, and 35% or so, viscosity 1000-1400mpa.s, comprehensive performance is seen below solid content
Table.
Embodiment 4
1. unsaturated fatty acid modified epoxy is prepared according to the raw material of following quality:By 250g epoxy resin E20 with
125g eleostearic acids are added in reaction bulb, and 200g dipropylenes are then added, and 1g triphenyl phosphorus is added, and high-speed stirred is equal
It is even, 120 DEG C or so are warming up to, is reacted 4 hours or so, then measures acid value, cooling stopping is anti-when acid value is less than the 5% of initial value
It answers；
2. the poly glycol monomethyl ether for the 400g that maleic anhydride 100g and molecular weight are 400 is added in reactor, 1g is added
Triethylamine, after stirring evenly, increase reaction temperature to 110 DEG C, reaction 3 hours after cooling discharge；
3. taking 250g to take the mixture in 550g steps 1 to be added to instead with the reactant in step 1 reactant in step 2
Answer in device, 1g tetrabutyl phosphate warmings while stirring be added to 100 DEG C, after reaction 4 hours, cool to 60 DEG C, dropwise addition go from
Sub- water 600g, after being added dropwise to complete, cooling discharge obtains the epoxy emulsion of one-component.
The lotion is yellow liquid, and 43% or so, viscosity 700-1200mpa.s, comprehensive performance is seen below solid content
Table.
Embodiment 5
1. unsaturated fatty acid modified epoxy is prepared according to the raw material of following quality:By 180g epoxy resin E54 with
280g oleic acid is added in reaction bulb, and 200g butyl glycol ethers are then added, and 1g triphenyl phosphorus is added, and high-speed stirred is uniform, is risen
Temperature is reacted 3 hours or so to 120 DEG C or so, then measures acid value, cooling stopping reaction when acid value is less than the 5% of initial value；
2. the poly glycol monomethyl ether for the 800g that maleic anhydride 100g and molecular weight are 800 is added in reactor, 1g is added
Triethylamine, after stirring evenly, increase reaction temperature to 120 DEG C, reaction 3 hours after cooling discharge；
3. taking 350g to take the mixture in 250g steps 1 to be added to instead with the reactant in step 1 reactant in step 2
Answer in device, 1g tetrabutyl phosphate warmings while stirring be added to 110 DEG C, after reaction 4 hours, cool to 60 DEG C, dropwise addition go from
Sub- water 500g, after being added dropwise to complete, cooling discharge obtains the epoxy emulsion of one-component.
The lotion is yellow liquid, and 45% or so, viscosity 500-900mpa.s, comprehensive performance see the table below solid content.
The obtained single-component epoxy lotion of 1 three kinds of embodiments of table and its coating property
Present invention gained single-component epoxy lotion has preferable storage stability it can be seen from table one, the paint film tool prepared
There are good adhesive force, hardness, the performances such as acid and alkali-resistance and salt fog, therefore the anti-corrosion primer of steel construction can be used to prepare.
For a further understanding of or verification the present invention prepared by product emulsion performance, by the lotion of embodiment 1 and 2 divide
It does not carry out preparing anti-corrosion primer and be tested, specially；
Embodiment 6
By 30 deionized waters and 6 parts of trbasic zinc phosphates, 3 parts of aluminum phosphates, 3 parts of iron oxide reds, 6 parts of precipitation method barium sulfate, 2 parts of micas, 0.1 part
Bentonite, 1 part of wetting agent, 0.2 antifoaming agent are added in grinder, are ground to fineness《After 30um, by this 40 parts of slurry tune
Enter in 60 parts of lotions in embodiment 1, and add 0.2 part of antifoaming agent, 0.2 part of wetting agent adds 4 parts of deionized waters, is transferred to conjunction
It discharges after suitable viscosity, specific performance is shown in Table 2.
Embodiment 7
By 30 deionized waters and 6 parts of trbasic zinc phosphates, 3 parts of aluminum phosphates, 3 parts of iron oxide reds, 6 parts of precipitation method barium sulfate, 2 parts of micas, 0.1 part
Bentonite, 1 part of wetting agent, 0.2 antifoaming agent are added in grinder, are ground to fineness《After 30um, by this 40 parts of slurry tune
Enter in 60 parts of lotions in embodiment 1, and add 0.2 part of antifoaming agent, 0.2 part of wetting agent adds 4 parts of deionized waters, is transferred to conjunction
It discharges after suitable viscosity, specific performance is shown in Table 2.
By embodiment 6 and embodiment 7 as can be seen that after paint is made in the single-component epoxy lotion prepared through the invention
It has excellent performance, and the coating storage stability prepared is preferable, can be used to prepare the anti-corrosion primer of steel substrate.
Claims (10)
1. the preparation method of aqueous one-component epoxy resin latex, feature include the following steps：
The synthesis of first step unsaturated fatty acid modified epoxy
It is calculated with molal quantity, by epoxy group molal quantity and unsaturated fatty acid molal quantity according to 1-1.2:1 ratio is added to instead
It answers in device, stirring solvent is then added at homogeneous, the catalyst for the 0.01-0.05 that molal quantity is epoxy group molal quantity is added,
It is warming up to 120-150 DEG C of progress esterification, after reacting 3-5 hours, it is eventually that the acid value of detection architecture, which is the 5% or less of initial value,
The epoxy resin that room temperature unsaturated fatty acid is modified is made in point；
Second step prepares anhydride modified hydrophilic segment
In order to solve the water-wet behavior of modified epoxy, the hydrophilic chain with carboxyl is prepared by esterification in this step
Section, it with molar ratio is 1 that specific implementation method, which is by the poly glycol monomethyl ether of acid anhydrides and number-average molecular weight 400-2000,:1-
0.8 in catalyst（Weight is the 0.05-0.1 of poly glycol monomethyl ether）The lower progress esterification of effect is prepared；
Above-mentioned esterification reaction temperature is at 80-120 DEG C, and reaction time of esterification was at 2-5 hours；
Third walks the preparation of aqueous one-component epoxy emulsion；
The anhydride modified hydrophilic segment that the epoxy resin that unsaturated fatty acid prepared by the first step is modified is prepared with second step
Esterification is carried out under the effect of the catalyst, is eventually adding the epoxy emulsion that deionized water is prepared into aqueous one-component.
2. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：The asphalt mixtures modified by epoxy resin
Fat is epoxy resin, the bisphenol-A obtained by epoxychloropropane or methyl epichlorohydrin and bisphenol-A, Bisphenol F or bisphenol sulphone
The polyglycidyl ether of epoxyalkane merchant Chengwu, the polyalcohols such as polypropylene glycol, 1,6- hexylene glycols, trimethylolpropane, glycerine
Polyglycidyl ether；The polycarboxylic poly glycidyl esters and poly epihydric alcohol amine etc. such as adipic acid, phthalic acid, dimer acid.
3. being more preferably selected from the above-mentioned epoxy resin or adipic acid prepared with epoxychloropropane with above-mentioned bisphenol-A or Bisphenol F
Polycarboxylic acid be modified made of epoxy resin.
4. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：The unsaturation
Aliphatic acid is selected from oleic acid（Octadecenoic acid）, linoleic acid siritch（18 carbon enoic acids）, leukotrienes（18 carbon enoic acids）, recklessly
At least one of sesame oil, tung oil, ricinoleic acid.
5. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：The solvent choosing
From the glycol dinitrates such as monoethylene glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, ethylene glycol monobutyl ether ethers and
Butyl ether class, ethylene glycol monobutyl ether；Propylene glycol monomethyl ether, propylene glycol monoethyl, glycol monobutyl ether, propylene glycol list isobutyl
At least one of propylene-glycol monoalky lethers classes such as base ether, propylene glycol list tertbutyl ether.
6. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：It is synthesized in the first step
Described in catalyst be selected from least one of butyl titanate, monomethyl tin oxide, triphenyl phosphorus and tetrabutylammonium bromide.
7. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：The acid anhydrides choosing
From at least one of phthalic anhydride, acetic anhydride, maleic anhydride, succinic anhydride, phthalic anhydride, o- benzoic acid acid anhydride
The preparation method of aqueous one-component epoxy resin latex according to right 1, it is characterised in that：The polyethylene glycol
Its number-average molecular weight of monomethyl ether is between 400-1000.
8. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：It is synthesized in second step
Described in catalyst be selected from triethylamine, tri-n-butylamine, benzyldimethylamine, 2,4,2,4,6- tri- (dimethylaminomethyl) phenol, N-
The tertiary amines such as methyl piperazine and its esters；2-methylimidazole, 2- phenylimidazoles, 2- undecyl imidazoles, 2- ethyl -4- methyl miaows
Azoles；Tetraphenyl microcosmic salt, methyl tributyl microcosmic salt, methyl tricyanoethyl microcosmic salt, at least one of tetrabutyl microcosmic salt.
9. the preparation method of the aqueous one-component epoxy resin latex according to right 1, it is characterised in that：It walks and synthesizes in third
Described in catalyst be selected from triethylamine, tri-n-butylamine, benzyldimethylamine, 2,4,2,4,6- tri- (dimethylaminomethyl) phenol, N-
The tertiary amines such as methyl piperazine and its esters；2-methylimidazole, 2- phenylimidazoles, 2- undecyl imidazoles, 2- ethyl -4- methyl miaows
Azoles；Tetraphenyl microcosmic salt, methyl tributyl microcosmic salt, methyl tricyanoethyl microcosmic salt, at least one of tetrabutyl microcosmic salt.
10. the preparation method of aqueous one-component epoxy resin latex, it is characterised in that it in claim 1-9 the methods by appointing
One kind is made.
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Application publication date: 20180821 |