CN103755966B - Emulsifying agent that aqueous solid epoxy resin latex is special and the preparation method of emulsion - Google Patents
Emulsifying agent that aqueous solid epoxy resin latex is special and the preparation method of emulsion Download PDFInfo
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- CN103755966B CN103755966B CN201410009262.4A CN201410009262A CN103755966B CN 103755966 B CN103755966 B CN 103755966B CN 201410009262 A CN201410009262 A CN 201410009262A CN 103755966 B CN103755966 B CN 103755966B
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Abstract
The present invention proposes the special emulsifying agent of a kind of aqueous solid epoxy resin latex and the preparation method of emulsion；We are with solid epoxy for emulsion matrix, and with polyetheramine and Aethoxy Sklerol as hydrophilic segment, liquid epoxies is oleophylic segment, prepares the block type emulsifying agent that aqueous solid epoxy resin latex is special.In conjunction with high speed dispersor, the manufacturing process such as nanometer emulsified machine, by shorter process time, obtain stable high solid content nanometer solid epoxy emulsion.High performance nanoscale solids epoxy resin latex prepared by this programme, has emulsification times short, and energy consumption is low, solid content high (40% 60%), the features such as particle diameter is little and dispersion is low (200nm 500nm), moderate viscosity (300mPa s 800mPa s), excellent in stability.Solve solid epoxy and be difficult to the problem of emulsifying, the problem of the emulsion film fragility that customer service is prepared with liquid epoxies for matrix.
Description
Technical field
The invention belongs to technical field of macromolecules, be specifically related to preparation and the nanoscale thereof of a kind of solid epoxy emulsifier special
The preparation method of solid epoxy emulsion.
Background technology
Along with the progress of social civilization, people there has also been higher requirement to coating technology and product.Since the seventies in last century
Since, polluting to protect environment to reduce, it is low that people have invented water paint, powdery paints, the contour performance of high solid coating
The coating variety polluted.Water paint is using water as solvent, is dispersed therein by synthetic resin, water paint environmental protection,
Nontoxic, there is no an abnormal smells from the patient, save resource, and with low cost, wide material sources, it is also possible to reduce safety in transit hidden
Suffer from.But compared to solvent based coating, water paint also has certain drawback.In order to make coating stabilization, usual formula can add
Multiple additives, and film performance tool is had a significant impact by these additives just, affects the performance of coating, the most corrosion-resistant
Performance, the most slowly, technology develops does not has big progress always in the development of water-based anticorrosive paint the most for a long time, but technology
Difficulty is relatively big, but the enthusiasm of water-based anticorrosive paint is not gone down by the whole world, also always works on all kinds of research, aqueous third
Olefin(e) acid coating, aqueous polyurethane coating, aqueous epoxy coating all present excellent performance, and in succession come into operation.
The traditional additional emulsifying agent of aqueous epoxy resin emulsion uses small-molecule substance, but the easy breakdown of emulsion of aqueous emulsion of preparation,
Unstable；And free little molecule causes coating film performance to decline, mainly decay resistance is greatly affected.Emulsion
Being thermodynamic instability system, its stability is by latex intergranular electrostatic force, Van der Waals force, solvation and interfacial tension etc.
The result of many factors comprehensive function, and can dispersion phase keep relative dynamic stable for a long time, emulsifying agent plays conclusive effect.
Have as hydrophilic segment, synthesis using epoxy molecule main chain as lipophilic fraction, hydrophilic group or the hydrophilic segment of grafting
The epoxy resin emulsifying agent of parents' performance, this kind of emulsifying agent is similar to the molecular structure of body epoxy resin, with epoxy resin compatibility
Property is good, thus can improve the stability of epoxy resin aqueous emulsion；In addition the epoxide group in emulsifying agent structure can be anti-with firming agent
Should, in stable existence and cured product, and outside being free on system unlike small-molecular emulsifier, film performance can be improved.
The aqueous epoxy resin emulsion used in current social, major part is that raw material is prepared, due to Breakup of Liquid Ring by liquid epoxy
Epoxy resins molecular weight is little, and epoxide number is high, and the crosslink density of the paint film that final cured coating film obtains is high, and fragility is big, corrosion-resistant,
Have a strong impact on its serviceability, cause the aqueous epoxy coating cannot spread.Therefore the emulsifying agent of solid epoxy is studied
Being significant with emulsification method, the report of current solid epoxy resin emulsifier special is almost nil, and this patent has filled up this
The blank of aspect.
Summary of the invention
The present invention provides the emulsifying agent that a kind of aqueous solid epoxy resin latex is special, and nanoscale solids epoxy resin latex
Preparation method.
We are with solid epoxy for emulsion matrix, and with polyetheramine and Aethoxy Sklerol as hydrophilic segment, liquid epoxies is oleophylic
Segment, prepares the block type emulsifying agent that aqueous solid epoxy resin latex is special.In conjunction with high speed dispersor, nanometer emulsified machine etc.
Manufacturing process, by shorter process time, obtains stable high solid content nanometer solid epoxy emulsion.
Technical scheme is as follows:
A kind of preparation method of the emulsifier special for aqueous solid epoxy resin latex, step is as follows:
(1) at 40-60 DEG C by liquid epoxies and polyethers according to mass ratio: 1:0.5-1:20 feeds intake；And at 40-60
Pre-hot mixing 10-30min at DEG C；
(2) adding catalyst at the 40-60 DEG C of mixture in step (1), catalyst amount is all rings in step (1)
3 ‰-the 3% of the quality sum of epoxy resins and polyethers, reacts 0.5h-2h at 40-60 DEG C；
(3) to 70-90 DEG C, the polyethers of the 10%-50% of the quality sum of all epoxy resin and polyethers in step (1) is added,
Reaction 0.5h-3h；Obtain block type or random emulsifying agent.
Described liquid epoxies be bisphenol-A be epoxy resin E54, E51, E44, E42, E35 or E31 one of which
Or two kinds.
Described polyethers is polyetheramine D-230, polyetheramine D-400, polyetheramine D-2000, Polyethylene Glycol 500-2000 or poly-third
One or both in glycol 2000-8000.
Described catalyst is the one in aluminum chloride, boron trifluoride diethyl etherate, alkyl aluminum or zinc alkyl.
Use the present invention emulsifying agent prepare water nano level solid epoxy emulsion method, step is as follows:
(1) emulsifying agent is mixed homogeneously with solid epoxy, with high speed dispersor stirring mixing 10-30min at 60-90 DEG C；
(2) it is kept stirring for, so that the speed mixed system of 10-30ml/min to add deionized water, until there is phase reversal, body
Being to be become oil-in-water by Water-In-Oil, whole process temperature keeps constant, for 80-95 DEG C；
(3) continuing system is carried out emulsifying, emulsification times is 0.5h-2h, constant at maintaining the temperature at 60-80 DEG C, it is thus achieved that aqueous
Nanoscale solids epoxy resin latex.
Described solid epoxy is bisphenol A epoxide resin E20, and block structure solid epoxy emulsifier special consumption is
The 5%-15% of solid epoxy quality.
The stirring condition of described high speed dispersor is: the stir speed (S.S.) of described step (1) is 500r/min-2000r/min, institute
The stir speed (S.S.) stating step (2) is 1000r/min-5000r/min；Described step (3) is carried out under the stirring of nanometer emulsified machine,
Stir speed (S.S.) is 10000r/min-20000r/min.
By the liquid-state epoxy resin of oleophylic and hydrophilic polyethers carry out ring-opening polymerisation, synthesis one has-A-B-A-B-A-B-,
Or the aqueous solid epoxy resin of-A-B-C-B-A-B-C-B-block structure or-A-B-C-D-A-C-B-D-C-D-disordered structure
Emulsion emulsifier special.Wherein-A-B-A-B-A-B-block structure emulsifier special is by a kind of epoxy resin and a kind of polyetheramine/poly-
Ether alcohol prepares；-A-B-C-B-A-B-C-B-block structure emulsifier special by a kind of epoxy resin and two kinds of polyetheramine/Aethoxy Sklerols or
Two kinds of epoxy resin of person and a kind of polyetheramine/Aethoxy Sklerol prepare-；A-B-C-D-A-C-B-D-C-D-disordered structure emulsifier special by
Two kinds of epoxy resin and two or three kinds of polyetheramine/Aethoxy Sklerol prepare.
High performance nanoscale solids epoxy resin latex prepared by this programme, has emulsification times short, and energy consumption is low, and solid content is high
(40%-60%), particle diameter is little and dispersion is low (200nm-500nm), moderate viscosity (300mPa s-800mPa s), stable
Property the feature such as excellent.
The present invention, with solid epoxy as matrix, prepares its emulsifier special, solves solid epoxy and is difficult to asking of emulsifying
Topic, the problem of the emulsion film fragility that customer service is prepared with liquid epoxies for matrix.The most whole process has without any
Machine solvent, for green environmental friendly coatings, technique is simple, it is easy to accomplish, process time is short, and energy consumption is low.
Detailed description of the invention
Below by example, the present invention is described in further detail:
Embodiment 1
1. the synthesis of aqueous solid epoxy resin latex emulsifier special
Will be equipped with agitator, condensing tube, the 2L four-hole boiling flask of thermometer is put in water-bath, is initially charged 300g liquid in four-hole boiling flask
Body epoxy resin E-35, is warmed up to 50 DEG C, adds 300g polyetheramine D-400, stirs 10min, makes both mix homogeneously.
In appeal mixed system, add 3g aluminum trichloride catalyst, keep the stir speed (S.S.) of 300r/min, react at 60 DEG C
0.5h。
It is warming up to 80 DEG C, is slowly added dropwise 300g polyetheramine D-400 with pipet, keep the stir speed (S.S.) of 300r/min, at 80 DEG C
Lower reaction 1h, can obtain-A-B-A-B-A-B-block type the emulsifying agent that aqueous solid epoxy resin latex is special.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 80 DEG C, add the water of 20g appeal
Property the special block type emulsifying agent of solid epoxy emulsion, stir 10min with high speed dispersor with the rotating speed of 1000r/min.
Stir speed (S.S.) is improved to 3000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 30ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 80 DEG C constant, finally add water inventory big
It is about 500g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 60 DEG C, with the stir speed (S.S.) emulsifying of 15000r/min
30min, can obtain required nano-solid epoxy resin latex.
Embodiment 2
1. the synthesis of aqueous solid epoxy resin latex emulsifier special
Will be equipped with agitator, condensing tube, the 5L four-hole boiling flask of thermometer is put in water-bath, is initially charged 100g liquid in four-hole boiling flask
Body epoxy resin E-44, is warmed up to 40 DEG C, adds 1000g polypropylene glycol 4000, stirs 20min, makes both mix homogeneously.
In appeal mixed system, add 30g zinc alkyl catalyst, keep the stir speed (S.S.) of 300r/min, react at 60 DEG C
2h
It is warming up to 90 DEG C, is slowly added dropwise 1000g polypropylene glycol 4000 with pipet, keep the stir speed (S.S.) of 300r/min,
React 2h at 90 DEG C ,-A-B-A-B-A-B-block type the emulsifying agent that aqueous solid epoxy resin latex is special can be obtained.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 90 DEG C, add the water of 30g appeal
Property the special block type emulsifying agent of solid epoxy emulsion, stir 10min in order to high speed dispersor with the rotating speed of 1000r/min.
Stir speed (S.S.) is improved to 3000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 10ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 90 DEG C constant, finally add water inventory big
It is about 200g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 70 DEG C, with the stir speed (S.S.) emulsifying 1h of 10000r/min,
Required nano-solid epoxy resin latex can be obtained.
Embodiment 3
1. the synthesis of aqueous solid epoxy resin latex emulsifier special
Will be equipped with agitator, condensing tube, the 2L four-hole boiling flask of thermometer is put in water-bath, is initially charged 200g in four-hole boiling flask
Liquid epoxies E-31 is warmed up to 60 DEG C, adds 500g polyetheramine D-2000, stirs 30min so that it is mix homogeneously.
In appeal mixed system, add 10g aluminum alkyl catalyst, keep the stir speed (S.S.) of 300r/min, react at 50 DEG C
1h。
It is warming up to 90 DEG C, is slowly added dropwise 500g Macrogol 2000 with pipet, keep the stir speed (S.S.) of 300r/min, at 90 DEG C
Lower reaction 1h, can obtain aqueous solid epoxy resin latex special-A-B-C-B-A-B-C-B-block type emulsifying agent.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 85 DEG C, add the water of 12g appeal
Property the special block type emulsifying agent of solid epoxy emulsion, stir 30min with high speed dispersor with the rotating speed of 1500r/min.
Stir speed (S.S.) is improved to 3000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 20ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 90 DEG C constant, finally add water inventory big
It is about 300g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 80 DEG C, with the stir speed (S.S.) emulsifying 1h of 15000r/min,
Required nano-solid epoxy resin latex can be obtained.
Embodiment 4
1. the synthesis of aqueous solid epoxy resin latex emulsifier special
Will be equipped with agitator, condensing tube, the 5L four-hole boiling flask of thermometer is put in water-bath, is initially charged 50g E-42 in four-hole boiling flask
With 50g E-51, it is warmed up to 55 DEG C, adds 1000g polypropylene glycol 8000, stir 30min so that it is mix homogeneously.
In appeal mixed system, add 30g boron trifluoride diethyl etherate catalyst, keep the stir speed (S.S.) of 300r/min, at 55 DEG C
Reaction 1.5h.
It is warming up to 90 DEG C, is slowly added dropwise 1000g polypropylene glycol 8000 with pipet, keep the stir speed (S.S.) of 300r/min, at 90 DEG C
Lower reaction 1.5h, can obtain-A-B-C-B-A-B-C-B-block type the emulsifying agent that aqueous solid epoxy resin latex is special.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 60 DEG C, add the water of 15g appeal
Property the special block type emulsifying agent of solid epoxy emulsion, stir 30min with high speed dispersor with the rotating speed of 2000r/min.
Stir speed (S.S.) is improved to 5000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 20ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 85 DEG C constant, finally add water inventory big
It is about 250g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 85 DEG C, with the stir speed (S.S.) emulsifying 0.5h of 20000r/min,
Required nano-solid epoxy resin latex can be obtained.
Embodiment 5
Will be equipped with agitator, condensing tube, the 2L four-hole boiling flask of thermometer is put in water-bath, is initially charged 50g E-35 in four-hole boiling flask
With 50g E-54, it is warmed up to 45 DEG C, adds 400g polyetheramine D-2000, stir 30min so that it is mix homogeneously.
In appeal mixed system, add 5g zinc alkyl catalyst, keep the stir speed (S.S.) of 300r/min, at 45 DEG C, react 1h.
It is warming up to 75 DEG C, is slowly added dropwise 400g polyetheramine D-2000 with pipet, keep the stir speed (S.S.) of 300r/min, at 75 DEG C
Lower reaction 0.5h, can obtain-A-B-C-B-A-B-C-B-block type the emulsifying agent that aqueous solid epoxy resin latex is special.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 80 DEG C, add the water of 10g appeal
Property the special block type emulsifying agent of solid epoxy emulsion, stir 15min with high speed dispersor with the rotating speed of 500r/min.
Stir speed (S.S.) is improved to 3000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 20ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 80 DEG C constant, finally add water inventory big
It is about 400g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 85 DEG C, with the stir speed (S.S.) emulsifying 1h of 10000r/min,
Required nano-solid epoxy resin latex can be obtained.
Embodiment 6
1. the synthesis of aqueous solid epoxy resin latex emulsifier special
Will be equipped with agitator, condensing tube, the 2L four-hole boiling flask of thermometer is put in water-bath, is initially charged 100g in four-hole boiling flask
Liquid epoxies E-44 and 200g liquid epoxies E-31 is warmed up to 60 DEG C, add 200g cetomacrogol 1000 and
400g polypropylene glycol 2000, stirs 30min so that it is mix homogeneously.
In appeal mixed system, add 10g boron trifluoride diethyl etherate catalyst, keep the stir speed (S.S.) of 300r/min, at 70 DEG C
Reaction 1h.
It is warming up to 85 DEG C, is slowly added dropwise 200g Polyethylene Glycol 500 with pipet, keep the stir speed (S.S.) of 300r/min, at 85 DEG C
Lower reaction 1h, can obtain aqueous solid epoxy resin latex special or-A-B-C-D-A-C-B-D-C-D-random emulsifying
Agent.
2. the preparation of water nano level solid epoxy emulsion
In the beaker of 1L, add 200g solid epoxy E-20, with heating mantle heats to 80 DEG C, add the water of 15g appeal
Property the special random emulsifying agent of solid epoxy emulsion, stir 20min with high speed dispersor with the rotating speed of 2000r/min.
Stir speed (S.S.) is improved to 5000r/min, deionized water is added in above-mentioned mixed system, directly with the speed of 20ml/min
To phase reversal occurs, system is become oil-in-water by Water-In-Oil, whole process keep temperature be 95 DEG C constant, finally add water inventory big
It is about 300g.
Above-mentioned oil-in-water system is transferred in nanometer emulsified machine, at 80 DEG C, with the stir speed (S.S.) emulsifying 1.5h of 20000r/min,
Required nano-solid epoxy resin latex can be obtained.
The invention is not limited in the technology described in embodiment, its description is illustrative, and nonrestrictive, this
Bright authority is defined in the claims, and can change according to the present invention based on those skilled in the art, the method such as restructuring obtains
Technology related to the present invention, all within protection scope of the present invention.
Claims (7)
1. a preparation method for the emulsifying agent that aqueous solid epoxy resin latex is special, is characterized in that step is as follows:
(1) at 40-60 DEG C by liquid epoxies and polyetheramine according to mass ratio: 1:0.5-1:20 feeds intake；And
Pre-hot mixing 10-30min at 40-60 DEG C；
(2) adding catalyst at the 40-60 DEG C of mixture in step (1), catalyst amount is all rings in step (1)
3 ‰-the 3% of the quality sum of epoxy resins and polyetheramine, reacts 0.5h-2h at 40-60 DEG C；
(3) to 70-90 DEG C, the poly-of the 10%-50% of the quality sum of all epoxy resin and polyetheramine in step (1) is added
Ether, reacts 0.5h-3h；Obtain block structure emulsifying agent.
2. the method for claim 1, it is characterized in that described catalyst be aluminum chloride, boron trifluoride diethyl etherate, alkyl aluminum or
One in zinc alkyl.
3. the method for claim 1, is characterized in that described block structure emulsifying agent is by a kind of epoxy resin and a kind of polyethers
-A-B-A-B-A-B-block structure the emulsifier special that amine prepares.
4. the method for claim 1, is characterized in that described block structure emulsifying agent is by a kind of epoxy resin and two kinds of polyethers
Amine or two kinds of epoxy resin and a kind of polyetheramine prepare--A-B-C-B-A-B-C-B-block structure emulsifier special.
5. the method for claim 1, it is characterized in that described disordered structure emulsifier special be by two kinds of epoxy resin and two or
Three kinds of polyetheramines prepare A-B-C-D-A-C-B-D-C-D-.
6. use emulsifying agent as claimed in claim 1 prepare aqueous solid epoxy resin latex method, it is characterized in that step is as follows:
(1) emulsifier special is mixed homogeneously with solid epoxy, with high speed dispersor stirring mixing at 60-90 DEG C
10-30min；
(2) it is kept stirring for, so that the speed mixed system of 10-30ml/min to add deionized water, until there is phase reversal, body
Being to be become oil-in-water by Water-In-Oil, whole process temperature keeps constant, for 80-95 DEG C；
(3) continuing system is carried out emulsifying, emulsification times is 0.5h-2h, constant at maintaining the temperature at 60-80 DEG C, it is thus achieved that aqueous
Nanoscale solids epoxy resin latex.
7. method as claimed in claim 4, is characterized in that the stirring condition of described high speed dispersor is: described step (1)
Stir speed (S.S.) is 500r/min-2000r/min, and the stir speed (S.S.) of described step (2) is 1000r/min-5000r/min；Described step
Suddenly (3) are carried out under the stirring of nanometer emulsified machine, and stir speed (S.S.) is 10000r/min-20000r/min.
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| CN101585922A (en) * | 2009-06-12 | 2009-11-25 | 深圳航天科技创新研究院 | Method of using block polyether to prepare epoxy emulsion |
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