CN102167885A - High-intensity urea-formaldehyde resin microcapsule and preparation method thereof - Google Patents
High-intensity urea-formaldehyde resin microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-intensity urea-formaldehyde resin microcapsule. Titanium dioxide or silicon dioxide inorganic nanoparticles with particle diameter of 10 to 50 nm are doped in the wall material of the microcapsule. A preparation method of the high-intensity urea-formaldehyde resin microcapsule comprises the following steps of: mixing urea and formaldehyde according to a molar ratio of the urea to the formaldehyde of 1:1.75; adjusting the pH value to 8.5 to 9.0; stirring at the constant temperature of between 70 and 75 DEG C for 1 hour; diluting by adding distilled water to obtain urea-formaldehyde prepolymer solution with mass concentration of 35 to 60 percent; taking 10 to 20 milliliters of the urea-formaldehyde prepolymer solution and adjusting the pH value to 4.0 to 4.2; reacting at the temperature of between 23 and 26 DEG C for 1 hour to obtain water-soluble urea-formaldehyde resin; dispersing the inorganic nanoparticles into an oil phase to prepare 0.04 to 0.2 mass percent of inorganic particle dispersion liquid; adding 40 milliliters of 7.3 mass percent of deionized water solution of a system modifier into the water-soluble urea-formaldehyde resin; adding 4.5 milliliters of inorganic particle dispersion liquid dropwise under stirring to form emulsion and then adjusting the pH value to 3.0 to 3.5; reacting at the temperature of between 23 and 26 DEG C for 1 hour; adding 0.3 to 3 grams of curing agent; heating the product to 45 to 50 DEG C; performing heat-preserving reaction for 2 hours; and performing suction-filtration and drying to obtain the urea-formaldehyde resin microcapsule, of which the wall material is doped with the inorganic nanoparticles.
Description
One, technical field
The invention belongs to fine chemistry industry and microcapsulary field, particularly a kind of high strength urea-formaldehyde resin microcapsule and preparation method thereof.
Two, background technology
Solid, liquid, gas or its mixture (core or capsule-core) of dispersiveness are wrapped in the small container with " nuclear-shell " structure natural or synthetic macromolecular material or the middle formation of inorganic materials (wall material or cyst wall), are called microcapsule.Microcapsulary starts from the thirties in 20th century, and beginning to be widely used in to produce but is after U.S. NCR Corp. prepared oil-containing gelatin microcapsule and used it for noncarbon recording paper nineteen fifty-three.Since microencapsulated product the insulation blocking of active ingredient, slowly-releasing, and aspect such as targeted drug tangible characteristic is arranged, thereby since it comes out, just enjoyed people's attention.As a kind of commercialization means with excellent properties, microcapsulary has been widely used in fields such as food, medicine, feed, agricultural chemicals, coating, printing ink, textile dyeing and finishing, catalyzer, tackiness agent, washing composition, makeup, sensitive materials.In recent years, microcapsulary is in the application of field of compound material such as phase change material, self-repair material, liquid-crystal display, electrophoresis showed, for the development of microcapsulary provides more wide application prospect.
Urea-formaldehyde resin is with low cost, and synthesis condition is simple, is to be used for one of wall material commonly used for preparing microcapsule.Yet urea-formaldehyde resin water tolerance, ageing resistance are poor, and shrinking percentage height during curing easily produces internal stress and causes and break, with cave in easily in the process of dry and the coating distortion and breaking of its microcapsule of making feedstock production.And because urea-formaldehyde resin and non-homogeneous successive Polymer Structure, there is micropore in microcapsule prepared therefrom on the cyst wall, cause the stopping property of microcapsule relatively poor, are unfavorable for the storage of inner core.
Usually can adopt urea-formaldehyde resin is carried out modification, prepares the stopping property and the anti-performance of caving in of the method for bilayer or multilayer microcapsule with the raising urea-formaldehyde resin microcapsule, but these method complicated process of preparation, and preparation process also is difficult to control.
Three, summary of the invention
Technical problem:
The object of the present invention is to provide a kind of high strength urea-formaldehyde resin microcapsule that can improve the capsule-wall physical strength and preparation method thereof.Solve that the urea-formaldehyde resin microcapsule stopping property is poor, easily cave in after the drying, the defective of cracky, solve complicated process of preparation simultaneously, be difficult to control, the difficult point of severe reaction conditions.
Technical scheme:
A kind of high strength urea-formaldehyde resin microcapsule of the present invention, this capsular wall material is the urea-formaldehyde resin that is doped with 2% ~ 7% inorganic nano-particle of wall material amount, and described inorganic nano-particle is that particle diameter is nano titanium oxide or the nano silicon of 10 ~ 50nm.
High strength Preparation of Urea-formaldehyde Microcapsule method of the present invention may further comprise the steps:
1) urea is mixed according to mol ratio 1:1.75 with formaldehyde, regulate its pH value to 8.5 ~ 9.0,70 ℃ ~ 75 ℃ of following constant temperature and stirred 1 hour, be cooled to room temperature, add distilled water diluting, promptly obtain mass concentration and be the urea aldehyde prepolymer solution of 35% ~ 60% clear
2) get the urea aldehyde prepolymer solution that 10 ~ 20mL step 1) obtains, regulate its pH value to 4.0 ~ 4.2,23 ℃ ~ 26 ℃ reaction 1 hour, promptly get water-soluble urea-formaldehyde resin,
3) inorganic nano-particle is scattered in to be mixed with mass percent in the oil phase be 0.04% ~ 0.2% inorganic particulate dispersion liquid, to step 2) add deionized water and the system's properties-correcting agent that 40mL contains system's properties-correcting agent in the water-soluble urea-formaldehyde resin that obtains and account for 7.3% of system's properties-correcting agent and deionized water total mass, stir and drip the inorganic particulate dispersion liquid that 4.5ml has prepared down again, regulate its pH value to 3.0 ~ 3.5 after forming emulsion, 23 ~ 26 ℃ of reactions added 0.3 ~ 3g solidifying agent after 1 hour, be warming up to 45 ~ 50 ℃, insulation reaction finished reaction in 2 hours, cooling, suction filtration is drying to obtain the urea-formaldehyde resin microcapsule that is doped with inorganic nano-particle in the wall material.
Inorganic nano-particle used in the present invention is that particle diameter is nano titanium oxide or the nano silicon of 10 ~ 50nm.
Oil phase used in the present invention is hexanaphthene, zellon or both mixtures.
System used in the present invention properties-correcting agent is sodium-chlor, gelatin and Resorcinol, and its mass ratio is 80:2.4:1.
Solidifying agent used in the present invention is an ammonium chloride.
The method of the invention is to be dispersed with inorganic nano-particle in oil phase, because its surface hydrophilicity, inorganic particulate can move to water-oil interface, in the urea-formaldehyde resin in-situ polymerization, inorganic nano-particle can because of and the active group on urea-formaldehyde resin surface between form interactions such as hydrogen bond, Van der Waals force and generation bonding, and be embedded among the cyst wall of microcapsule, thereby improved the physical strength of microcapsule cyst walls.Simultaneously, the introducing of inorganic nano-particle can effectively reduce the quantity of surface of microcapsule micropore, thereby improves the compactness of microcapsule wall, improves the stability in storage of core in the microcapsule.
Beneficial effect:
React according to technique scheme: reaction conditions gentleness, preparation technology are simple relatively, and be easy to control; Not damaged after the microcapsule regular shape that is doped with inorganic nano-particle for preparing, smooth surface, the drying, as not cave in, have excellence sealing property.
Among the present invention, the inorganic nano-particle that in the wall material of the urea-formaldehyde resin microcapsule for preparing, mixed, there is the hydroxyl of a large amount of unsaturated residual bonds and different bonding states on its surface, is easy to hydroxyl or amino hydrogen bond or the Van der Waals force of forming with urea-formaldehyde resin.Simultaneously because the surface effects and the small-size effect of inorganic nano-particle makes it have higher surface energy, the serious coordination deficiency in surface, easily and the active group in the urea-formaldehyde resin play bonding action.Therefore, inorganic nano-particle is not simple and urea-formaldehyde resin blend, but is intertwined with the urea-formaldehyde resin polymer molecular chain, finally is embedded in the middle of the wall material of urea-formaldehyde resin microcapsule.Because enhancing, the toughening effect of inorganic nano-particle, the physical strength of resulting microcapsule cyst wall also is improved.Meanwhile, the introducing of inorganic nano-particle can also effectively reduce the quantity of surface of microcapsule micropore, thereby improves the compactness of microcapsule wall, improves the stability in storage of core in the microcapsule.
In the present invention, select for use sodium-chlor, gelatin and Resorcinol to mix as system's properties-correcting agent by the certain mass ratio.The adding of sodium-chlor can increase oil water interfacial tension, promotes urea-formaldehyde resin in the coalescent enrichment of water-oil interface, thereby forms fine and close microcapsule.Gelatin and Resorcinol can be controlled the coagulation speed of urea-formaldehyde resin micelle and the plasticity and the viscosity of microcapsule cyst wall, thereby improve the surface flatness and the compactness of microcapsule.
In the present invention, select for use ammonium chloride to make solidifying agent,, can control the speed of response of ammonium chloride and formaldehyde, obtain smooth surface, be doped with the urea-formaldehyde resin microcapsule of inorganic nano-particle in not damaged after the drying, the cyst wall that do not cave in by transferring the knot solidification value.
Four, description of drawings
Fig. 1 is the sem photograph of the product that made by the present invention.
Fig. 2 is the X-ray energy spectrum figure of the product that made by the present invention.
Fig. 3 is the optical microscope photograph of the product that made by the present invention.
Fig. 4 is the optical microscope photograph that does not contain the urea-formaldehyde resin microcapsule of inorganic nano-particle in the cyst wall.
Fig. 5 is the stereoscan photograph that does not contain the urea-formaldehyde resin microcapsule of inorganic nano-particle in the cyst wall.
Five, embodiment
Embodiment 1
A kind of high strength urea-formaldehyde resin microcapsule, this capsular wall material is the urea-formaldehyde resin that is doped with 2%, 3%, 5%, 7% inorganic nano-particle of wall material amount, and described inorganic nano-particle is that particle diameter is nano titanium oxide or the nano silicon of 10nm, 20nm, 30nm, 50nm.
Embodiment 2
A kind of high strength Preparation of Urea-formaldehyde Microcapsule method may further comprise the steps:
1) urea is mixed according to mol ratio 1:1.75 with formaldehyde, regulate its pH value to 8.5,8.7 or 9.0,70 ℃, 73 ℃ or 75 ℃ of following constant temperature stirred 1 hour, be cooled to room temperature, add distilled water diluting, obtain mass concentration and be the urea aldehyde prepolymer solution of 35%, 45%, 60% clear
2) get the above-mentioned urea aldehyde of 10mL, 13mL, 15mL or 20mL prepolymer solution, regulate its pH value to 4.0,4.1 or 4.2,23 ℃, 25 ℃ or 26 ℃ of reactions 1 hour, promptly get water-soluble urea-formaldehyde resin,
3) get 0.01,0.03 or the 0.05g inorganic nano-particle is scattered in, and to be mixed with mass percent in the oil phase be 0.04%, 0.12% or 0.2% inorganic particulate dispersion liquid, to step 2) add deionized water and the system's properties-correcting agent that 40mL contains system's properties-correcting agent in the water-soluble urea-formaldehyde resin that obtains and account for 7.3% of system's properties-correcting agent and deionized water total mass, stir and drip the inorganic particulate dispersion liquid that 4.5ml has prepared down, regulate its pH value to 3.0 after forming emulsion, 3.2 or 3.5,23 ℃, 25 ℃ or 26 ℃ reaction added 0.3 after 1 hour, 1.5 or 3g solidifying agent, be warming up to 45 ℃ or 50 ℃, insulation reaction finished reaction in 2 hours, cooling, suction filtration is drying to obtain the urea-formaldehyde resin microcapsule that is doped with inorganic nano-particle in the wall material.
In the present embodiment,
Employed inorganic nano-particle is that particle diameter is nano titanium oxide or the nano silicon of 10nm, 20nm, 30nm or 50nm.
Employed oil phase is hexanaphthene, zellon or both mixtures.
Employed system properties-correcting agent is made up of sodium-chlor, gelatin and Resorcinol, and its mass ratio is 80:2.4:1.
Employed solidifying agent is an ammonium chloride.
Comparative Examples:
Adopt to prepare microcapsule with the foregoing description 2 identical methods, difference is not add inorganic nano-particle in the reaction.Measurement result is shown in Fig. 4 and Fig. 5.Can find that by the microcapsule (Fig. 1 and Fig. 3) that are added with nano titanium oxide in the contrast cyst wall adding of inorganic nano-particle has improved the compactness of urea resin microcapsule wall and the stability in storage of the interior core of capsule.
With reference to Fig. 1 and Fig. 5, spherical full according to scanning electron microscope picture analysis revealed product of the present invention (Fig. 1), do not cave in after the drying, not damaged, and the microcapsule (Fig. 5) that do not add inorganic nano-particle in the cyst wall have much and cave in, are out of shape, prove product of the present invention, compare with the microcapsule that do not add inorganic nano-particle in the cyst wall, the physical strength height of cyst wall is difficult for caving in and being out of shape.
With reference to Fig. 2, according to X-ray energy spectrum analysis revealed product of the present invention, the Ti element is arranged in its cyst wall, prove in the product cyst wall to be doped with nano titanium oxide.
With reference to Fig. 3 and Fig. 4, storage characteristics according to core in light micrograph analysis revealed product of the present invention (Fig. 3) capsule is better, easy to leak not, and the microcapsule (Fig. 4) that do not add inorganic nano-particle in the cyst wall have a lot of capsulae vacuuses to occur after drying, prove product of the present invention, compare with the microcapsule that do not add inorganic nano-particle in the cyst wall, have excellent stopping property.
Claims (6)
1. high strength urea-formaldehyde resin microcapsule, it is characterized in that, this capsular wall material is the urea-formaldehyde resin that is doped with 2% ~ 7% inorganic nano-particle of wall material amount, and described inorganic nano-particle is that particle diameter is nano titanium oxide or the nano silicon of 10 ~ 50nm.
2. the described high strength Preparation of Urea-formaldehyde Microcapsule of claim 1 method is characterized in that, may further comprise the steps:
Urea is mixed according to mol ratio 1:1.75 with formaldehyde, regulates its pH value to 8.5 ~ 9.0,70 ℃ ~ 75 ℃ of following constant temperature and stirred 1 hour, be cooled to room temperature, add distilled water diluting, promptly obtain mass concentration and be the urea aldehyde prepolymer solution of 35% ~ 60% clear,
Get the urea aldehyde prepolymer solution that 10 ~ 20mL step 1) obtains, regulate its pH value to 4.0 ~ 4.2,23 ℃ ~ 26 ℃ reaction 1 hour, promptly get water-soluble urea-formaldehyde resin,
Inorganic nano-particle is scattered in to be mixed with mass percent in the oil phase be 0.04% ~ 0.2% inorganic particulate dispersion liquid, to step 2) add deionized water and the system's properties-correcting agent that 40mL contains system's properties-correcting agent in the water-soluble urea-formaldehyde resin that obtains and account for 7.3% of system's properties-correcting agent and deionized water total mass, stir and drip the inorganic particulate dispersion liquid that 4.5ml has prepared down again, regulate its pH value to 3.0 ~ 3.5 after forming emulsion, 23 ~ 26 ℃ of reactions added 0.3 ~ 3g solidifying agent after 1 hour, be warming up to 45 ~ 50 ℃, insulation reaction finished reaction in 2 hours, cooling, suction filtration is drying to obtain the urea-formaldehyde resin microcapsule that is doped with inorganic nano-particle in the wall material.
3. preparation method according to claim 2 is characterized in that employed inorganic nano-particle is that particle diameter is nano titanium oxide or the nano silicon of 10 ~ 50nm.
4. preparation method according to claim 2 is characterized in that employed oil phase is hexanaphthene, zellon or both mixtures.
5. preparation method according to claim 2 is characterized in that employed system properties-correcting agent is made up of sodium-chlor, gelatin and Resorcinol, and its mass ratio is 80:2.4:1.
6. preparation method according to claim 2 is characterized in that employed solidifying agent is an ammonium chloride.
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Application publication date: 20110831 |