CN109370153A - A kind of aqueous epoxy emulsion and preparation method thereof reacted that can mix with oiliness curing agent - Google Patents
A kind of aqueous epoxy emulsion and preparation method thereof reacted that can mix with oiliness curing agent Download PDFInfo
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- CN109370153A CN109370153A CN201811172168.5A CN201811172168A CN109370153A CN 109370153 A CN109370153 A CN 109370153A CN 201811172168 A CN201811172168 A CN 201811172168A CN 109370153 A CN109370153 A CN 109370153A
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of aqueous epoxy emulsions reacted that can mix with oiliness curing agent, in parts by weight, including following components: 50-70 parts of epoxy resin E51-128;4-8 parts of emulsifier;1-3 parts of thickener;0.1-0.5 parts of defoaming agent;30-50 parts of deionized water;The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is (3-5): (1-3);The reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier.The invention also discloses the preparation methods of the aqueous epoxy resin emulsion.This method is easy to operate, and preparation cost is low, good emulsion stability obtained, good with aqueous/oiliness curing agent intermiscibility, and reacts comprehensively with oiliness curing agent, and completion of cure, performance is good after solidification.
Description
Technical field:
The present invention relates to the preparation fields of epoxy emulsion, are specifically related to a kind of water reacted that can mix with oiliness curing agent
Property epoxy emulsion and preparation method thereof.
Background technique:
Epoxy resin has excellent adhesion, thermal stability, chemical-resistant, insulating properties and mechanical strength etc., extensively
Applied to fields such as coating, adhesive and composite materials.But common epoxy resin be it is water-insoluble, be only soluble in aromatic hydrocarbons,
The organic solvents such as alcohols and ketone will cause pollution to environment.With the enhancing of global environmental consciousness, national governments are increasingly heavier
Pollution depending on volatile organic matter to environment.China is also in implementation on July 1st, 2004 coating environmental protection standard.So to asphalt mixtures modified by epoxy resin
The Water-borne modification of rouge has become hot spot studied both at home and abroad at present.
Currently, existing aqueous epoxy resins majority is that the simple Phase inversion emulsification of oiliness epoxy resin forms in the market, it can only
It is used cooperatively with waterborne curing agent, and with oiliness curing agent there are intermiscibility is bad, react not comprehensive, performance difference etc. is asked after solidification
Topic.
Summary of the invention:
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of can mix with oiliness curing agent to react aqueous
Epoxy emulsion, the stable system is good with aqueous/oiliness curing agent intermiscibility, and reacts comprehensively with oiliness curing agent, has solidified
Entirely, performance is good after solidification.
The invention also discloses the preparation methods of the aqueous epoxy emulsion.
To achieve the above object, the invention adopts the following technical scheme:
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is (3-5): (1-
3);Other type emulsifiers are the surfactant that can make to be formed stable emulsion when two kinds of immiscible liquid mixing,
Its Water-borne modification that epoxy resin can be improved and the stability for increasing emulsion system;
The reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier, preparation method are as follows:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
It is to slowly warm up to 100-120 DEG C, back flow reaction 1-5h;It is cooled to room temperature, is then added dropwise just into reaction system after reaction
Silester is warming up to 130-150 DEG C, continues back flow reaction 5-10h, is cooled to room temperature after reaction, filters, and precipitating is successively
It is washed with deionized water and dehydrated alcohol, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;
(2) p-methyl benzenesulfonic acid and deionized water are mixed and p-methyl benzenesulfonic acid solution is made, be then added above-mentioned
Modified nano silicon oxide/hydroxyapatite composite material obtained, is stirred 10-40min, filters, freeze-drying, is made negative
Supported catalyst;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 75-90 DEG C, support type obtained above is then added
Catalyst is stirred 3-5min, and maleic anhydride is then added, and reacts 1-4h, filters while hot after reaction, and it is heavy to remove solid
It forms sediment, liquid is cooled to room temperature, filter, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier.
As a preferred embodiment of the above technical solution, the thickener is modified polyurethane thickener.
As a preferred embodiment of the above technical solution, in step (1), the hydroxyapatite, stearoyl keto isopropyl Aluminate,
The mass ratio of ethyl orthosilicate is 3:0.02:(0.1-0.6).
As a preferred embodiment of the above technical solution, in step (2), the mass concentration of the p-methyl benzenesulfonic acid solution is 5-
13%.
As a preferred embodiment of the above technical solution, in step (2), the modified nano silicon oxide/hydroxyapatite composite wood
The mass ratio of material and p-methyl benzenesulfonic acid solution is 1:(8-15).
As a preferred embodiment of the above technical solution, in step (3), the aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride
Molar ratio be (1-1.5): 1.
As a preferred embodiment of the above technical solution, in step (3), the aliphatic alcohol polyethenoxy class emulsifier, support type are urged
The mass ratio of agent is 5:(0.15-0.3).
A kind of preparation method for the aqueous epoxy emulsion reacted that can mix with oiliness curing agent, comprising the following steps:
Epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, is stirred,
Then be added other type emulsifiers, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, be eventually adding thickener and
Defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
As a preferred embodiment of the above technical solution, other described type emulsifiers are added in 15-20min.
As a preferred embodiment of the above technical solution, the revolving speed of the low speed dispersion is 500-800 revs/min.
The invention has the following advantages:
The present invention selects modified fatty alcohol polyethenoxy class emulsifier and other kinds of in aqueous epoxy resin emulsion
Emulsifier compounding be used as emulsifier, aliphatic alcohol polyethenoxy class emulsifier therein can effecting reaction emulsion epoxy resin, make to set
Rouge Water-borne modification, other type emulsifiers can be improved the Water-borne modification of epoxy resin and increase the stability of emulsion system, so that being made
Aqueous epoxy resin emulsion can not only mix with waterborne curing agent, and also there is preferable intermiscibility with oil-soluble curing agent;
For the modified fatty alcohol polyethenoxy class emulsifier that processability is excellent, the present invention is original with hydroxyapatite
Material is modified it using stearoyl keto isopropyl Aluminate first so that porous hydroxyapatite surface grafting have it is more
Active group;Then ethyl orthosilicate is added dropwise into system, reacts and modified nano silicon oxide/hydroxyapatite composite wood is made
Material, effectively improves the intensity of hydroxyapatite;The present invention is using it as carrier, using p-methyl benzenesulfonic acid as catalyst, is made negative
Supported catalyst, and under loaded catalyst obtained effect, using maleic anhydride to aliphatic alcohol polyethenoxy class emulsifier
Be modified, the catalyst activity is high, be made modified fatty alcohol polyethenoxy class emulsifier can effective emulsion epoxy resin,
Aqueous epoxy resin emulsion stability obtained is good, good with aqueous/oiliness curing agent intermiscibility.
Detailed description of the invention:
Fig. 1: aqueous epoxy emulsion made from the embodiment of the present invention 2 and commercially available ordinary emulsion in centrifuge 4500rpm,
The separation situation of sample emulsion in test tube is observed in centrifugation after twenty minutes;
Fig. 2: it is made in lotion and commercially available ordinary emulsion in the embodiment of the present invention 2 and is separately added into different oiliness solidifications
Agent stirs well even, the static stability for observing mixed liquor after twenty minutes by blender.
Specific embodiment:
For a better understanding of the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 3:1.5;It is described
Reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
100 DEG C are to slowly warm up to, back flow reaction 1h;It is cooled to room temperature after reaction, positive silicic acid second is then added dropwise into reaction system
Ester, is warming up to 130 DEG C, continues back flow reaction 5h, is cooled to room temperature after reaction, filters, precipitating successively with deionized water and
Dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxyapatite,
Stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.1;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 5% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 10min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:8;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 75 DEG C, support type obtained above is then added and urges
Agent is stirred 3min, and maleic anhydride is then added, and reacts 1h, filters while hot after reaction, removes solid precipitating, will
Liquid is cooled to room temperature, and filtering, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein, the rouge
Fat alcohol polyoxyethylene emulsifier, maleic anhydride molar ratio be 1:1;The aliphatic alcohol polyethenoxy class emulsifier, support type
The mass ratio of catalyst is 5:0.15;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Embodiment 2
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 4.5:2;It is described
Reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
120 DEG C are to slowly warm up to, back flow reaction 5h;It is cooled to room temperature after reaction, positive silicic acid second is then added dropwise into reaction system
Ester, is warming up to 150 DEG C, continues back flow reaction 10h, is cooled to room temperature after reaction, filters, precipitating successively with deionized water and
Dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxyapatite,
Stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.6;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 13% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 40min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:15;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 90 DEG C, support type obtained above is then added and urges
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 4h, filters while hot after reaction, removes solid precipitating,
Liquid is cooled to room temperature, is filtered, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein, described
Aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be 1.5:1;The aliphatic alcohol polyethenoxy class emulsifier is born
The mass ratio of supported catalyst is 5:0.3;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Embodiment 3
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 3:1.5;It is described
Reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
105 DEG C are to slowly warm up to, back flow reaction 2h;It is cooled to room temperature after reaction, positive silicic acid second is then added dropwise into reaction system
Ester, is warming up to 135 DEG C, continues back flow reaction 6h, is cooled to room temperature after reaction, filters, precipitating successively with deionized water and
Dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxyapatite,
Stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.2;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 7% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 20min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:10;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 80 DEG C, support type obtained above is then added and urges
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 2h, filters while hot after reaction, removes solid precipitating,
Liquid is cooled to room temperature, is filtered, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein, described
Aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be 1.1:1;The aliphatic alcohol polyethenoxy class emulsifier is born
The mass ratio of supported catalyst is 5:0.2;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Embodiment 4
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 3.5:1.5;Institute
Stating reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
110 DEG C are to slowly warm up to, back flow reaction 3h;It is cooled to room temperature after reaction, positive silicic acid second is then added dropwise into reaction system
Ester, is warming up to 140 DEG C, continues back flow reaction 7h, is cooled to room temperature after reaction, filters, precipitating successively with deionized water and
Dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxyapatite,
Stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.3;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 10% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 20min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:11;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 80 DEG C, support type obtained above is then added and urges
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 3h, filters while hot after reaction, removes solid precipitating,
Liquid is cooled to room temperature, is filtered, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein, described
Aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be 1.2:1;The aliphatic alcohol polyethenoxy class emulsifier is born
The mass ratio of supported catalyst is 5:0.2;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Embodiment 5
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 4:2;It is described anti-
Answering type emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
110 DEG C are to slowly warm up to, back flow reaction 4h;It is cooled to room temperature after reaction, positive silicic acid second is then added dropwise into reaction system
Ester, is warming up to 140 DEG C, continues back flow reaction 8h, is cooled to room temperature after reaction, filters, precipitating successively with deionized water and
Dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxyapatite,
Stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.4;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 12% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 30min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:12;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 85 DEG C, support type obtained above is then added and urges
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 3h, filters while hot after reaction, removes solid precipitating,
Liquid is cooled to room temperature, is filtered, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein, described
Aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be 1.3:1;The aliphatic alcohol polyethenoxy class emulsifier is born
The mass ratio of supported catalyst is 5:0.25;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Embodiment 6
A kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, in parts by weight, including following components:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is 4:1;It is described anti-
Answering type emulsifier is modified fatty alcohol polyethenoxy class emulsifier;
The preparation method of the aqueous epoxy emulsion the following steps are included:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate are then added, triethylamine is added dropwise,
115 DEG C are to slowly warm up to, back flow reaction 4.5h;It is cooled to room temperature after reaction, positive silicic acid is then added dropwise into reaction system
Ethyl ester is warming up to 140 DEG C, continues back flow reaction 9h, is cooled to room temperature after reaction, filters, and precipitating successively uses deionized water
It is washed with dehydrated alcohol, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;Wherein, the hydroxy-apatite
Stone, stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:0.5;
(2) p-methyl benzenesulfonic acid and the obtained mass concentration of deionized water mixing is molten for 12% p-methyl benzenesulfonic acid
Then liquid is added modified nano silicon oxide/hydroxyapatite composite material obtained above, is stirred 30min, filtering, cold
Dry, obtained loaded catalyst is lyophilized;Wherein, the modified nano silicon oxide/hydroxyapatite composite material with to methylbenzene
The mass ratio of sulfonic acid solutions is 1:13;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 85 DEG C, support type obtained above is then added and urges
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 3.5h, filters while hot after reaction, and it is heavy to remove solid
It forms sediment, liquid is cooled to room temperature, filter, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier;Wherein,
The aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be 1.4:1;The aliphatic alcohol polyethenoxy class emulsification
Agent, loaded catalyst mass ratio be 5:0.3;
(4) epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, stirred
It mixes, other type emulsifiers is then added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener
And defoaming agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
Performance test is done to aqueous epoxy emulsion obtained above below.Wherein No. 1 sample is made for the embodiment of the present invention 2
Aqueous epoxy emulsion, No. 2 samples are commercially available ordinary emulsion, and No. 2 samples are commercially available ordinary emulsion.
1, stability of emulsion:
The separation situation of sample emulsion in test tube is observed in centrifuge 4500rpm, centrifugation after twenty minutes: as can be seen from Figure 1: No. 1
Sample is substantially without separation;No. 2 20% clear liquids of sample;No. 3 samples are up to 60% clear liquid, here it is apparent that No. 1 sample stability is best.
2, lotion intermiscibility:
Be added different oiliness curing agent in lotion, stirred well by blender it is even, it is static to observe mixed liquor after twenty minutes
Stability.Figure it is seen that No. 1 sample, is precipitated without oiliness curing agent substantially, 2, No. 3 samples (universal lotion) have obvious oiliness
Curing agent is precipitated.
Claims (10)
1. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent, which is characterized in that in parts by weight, including it is following
Component:
The emulsifier is the mixing of reactive emulsifier and other type emulsifiers, and the two mass ratio is (3-5): (1-3);
The reactive emulsifier is modified fatty alcohol polyethenoxy class emulsifier, preparation method are as follows:
(1) hydroxyapatite and hexamethylene are mixed, stearoyl keto isopropyl Aluminate is then added, triethylamine is added dropwise, slowly
It is warming up to 100-120 DEG C, back flow reaction 1-5h;It is cooled to room temperature after reaction, positive silicic acid is then added dropwise into reaction system
Ethyl ester is warming up to 130-150 DEG C, continues back flow reaction 5-10h, is cooled to room temperature after reaction, filters, and precipitating is successively spent
Ionized water and dehydrated alcohol washing, it is dry, modified nano silicon oxide/hydroxyapatite composite material is made;
(2) p-methyl benzenesulfonic acid and deionized water are mixed and p-methyl benzenesulfonic acid solution is made, above-mentioned be made then is added
Modified nano silicon oxide/hydroxyapatite composite material, be stirred 10-40min, filter, freeze-drying, be made support type
Catalyst;
(3) aliphatic alcohol polyethenoxy class emulsifier is to slowly warm up to 75-90 DEG C, supported catalyst obtained above is then added
Agent is stirred 3-5min, and maleic anhydride is then added, and reacts 1-4h, filters while hot after reaction, removes solid precipitating,
Liquid is cooled to room temperature, is filtered, precipitating drying obtained obtains modified fatty alcohol polyethenoxy class emulsifier.
2. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that institute
Stating thickener is modified polyurethane thickener.
3. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that step
Suddenly in (1), the hydroxyapatite, stearoyl keto isopropyl Aluminate, ethyl orthosilicate mass ratio be 3:0.02:(0.1-
0.6)。
4. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that step
Suddenly in (2), the mass concentration of the p-methyl benzenesulfonic acid solution is 5-13%.
5. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that step
Suddenly in (2), the mass ratio of the modified nano silicon oxide/hydroxyapatite composite material and p-methyl benzenesulfonic acid solution is 1:
(8-15)。
6. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that step
Suddenly in (3), the aliphatic alcohol polyethenoxy class emulsifier, maleic anhydride molar ratio be (1-1.5): 1.
7. a kind of aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1, which is characterized in that step
Suddenly in (3), the aliphatic alcohol polyethenoxy class emulsifier, loaded catalyst mass ratio be 5:(0.15-0.3).
8. a kind of preparation method for the aqueous epoxy emulsion reacted that can mix with oiliness curing agent as described in claim 1,
It is characterized in that, comprising the following steps:
Epoxy resin E51-128, reactive emulsifier are mixed to join in blender, are heated to 40-50 DEG C, is stirred, then
Other type emulsifiers are added, adjusting speed of agitator is 1500 revs/min, is uniformly mixed, is eventually adding thickener and defoaming
Agent, low speed disperse 3-5min, and deionized water stirring is added, aqueous epoxy emulsion is made.
9. a kind of preparation method for the aqueous epoxy emulsion reacted that can mix with oiliness curing agent as claimed in claim 8,
It is characterized in that, other described type emulsifiers are added in 15-20min.
10. a kind of preparation method for the aqueous epoxy emulsion reacted that can mix with oiliness curing agent as claimed in claim 8,
It is characterized in that, the revolving speed of the low speed dispersion is 500-800 revs/min.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810387494 | 2018-04-26 | ||
CN2018103874941 | 2018-04-26 |
Publications (1)
Publication Number | Publication Date |
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CN109370153A true CN109370153A (en) | 2019-02-22 |
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CN114231122A (en) * | 2021-12-21 | 2022-03-25 | 天津科瑞达涂料化工有限公司 | Long-acting cold and hot water resistant water-based anticorrosive coating for inner wall of cast pipe and application thereof |
Citations (3)
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JPS5015487B1 (en) * | 1970-10-16 | 1975-06-05 | ||
CN101338064A (en) * | 2007-07-02 | 2009-01-07 | 深圳市海川实业股份有限公司 | Liquid epoxy resins emulsion and water-soluble epoxy terrace coating prepared thereby |
CN101463180A (en) * | 2007-12-19 | 2009-06-24 | 中国科学院广州化学研究所 | Aqueous single-component external emulsion epoxy resin emulsion and preparation thereof |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS5015487B1 (en) * | 1970-10-16 | 1975-06-05 | ||
CN101338064A (en) * | 2007-07-02 | 2009-01-07 | 深圳市海川实业股份有限公司 | Liquid epoxy resins emulsion and water-soluble epoxy terrace coating prepared thereby |
CN101463180A (en) * | 2007-12-19 | 2009-06-24 | 中国科学院广州化学研究所 | Aqueous single-component external emulsion epoxy resin emulsion and preparation thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114231122A (en) * | 2021-12-21 | 2022-03-25 | 天津科瑞达涂料化工有限公司 | Long-acting cold and hot water resistant water-based anticorrosive coating for inner wall of cast pipe and application thereof |
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