CN102965196B - Preparation method of essential-oil-coated urea-modified melamine resin microcapsules - Google Patents
Preparation method of essential-oil-coated urea-modified melamine resin microcapsules Download PDFInfo
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- CN102965196B CN102965196B CN201210445646.1A CN201210445646A CN102965196B CN 102965196 B CN102965196 B CN 102965196B CN 201210445646 A CN201210445646 A CN 201210445646A CN 102965196 B CN102965196 B CN 102965196B
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Abstract
The invention discloses a preparation method of essential-oil-coated urea-modified melamine resin microcapsules, which comprises the following steps: (1) wall material pre-crosslinking: by using a melamine-formaldehyde prepolymer as a wall material and urea as a modifier, carrying out pre-crosslinking to obtain a pre-crosslinked wall material solution; (2) core material emulsification: by using essential oil as a core material, forming an oil-in-water emulsion with the pre-crosslinked wall material solution; (3) capsule wall formation: stirring the oil-in-water emulsion to form capsule walls; and (4) termination of crosslinking reaction: adding an alkali solution to terminate the crosslinking reaction. The essential-oil-coated urea-modified melamine resin microcapsules prepared according to the method disclosed by the invention has the advantages of enhanced toughness, lower brittleness and improved storage stability, and slow release of the essential-oil in the microcapsules is facilitated; and the essential-oil-coated urea-modified melamine resin microcapsules have low formaldehyde residue level and favorable dispersity in the water-based solution system, and thus, is beneficial to application in washing agents and the like.
Description
Technical field
The present invention relates to microcapsules technology field, particularly a kind of preparation method of urea modification melamine resin microcapsules of coated essential oil.
Background technology
Material of microencapsulation technology permission is encapsulated in one and has size ranges in one micron of microballoon or micro-capsule arriving between hundreds of micron.This technology has been widely used in many-sided application such as medicine, agricultural, food, printing, cosmetics, daily use chemicals.
Along with the raising of expanding economy and people's living standard, people are greatly improved to the requirement of washing agent.When pursuing practical value, also to enjoyment, health direction, change gradually.In washing agent, add essential oil and can make clothing etc. retain fragrance, can make clothing anti-bacteria growth, covering smell, make people's body and mind comfortable.But essential oil, because volatility is very strong, is unfavorable for the reservation of washing agent fragrance.Utilize microcapsules technology, essential oil microencapsulation is joined in washing agent and can guarantee that essential oil is stable in storage process, on the other hand, in washing process, the microcapsules of the coated essential oil of part break essential oil are discharged through washing extruding, or stick in clothes fiber and continue slowly to discharge essential oil, make clothing retain for a long time fragrance.
Melamine resin, due to cheap, has good film-forming quality, is therefore widely used in the preparation of microcapsules.But melamine resin, because of its unique triazine ring and the interlaced structure of methylol, makes the microcapsules of preparation have the shortcomings such as poor toughness, fragility is high, bin stability is poor.In addition, because preparation process has been used formaldehyde, its residual quantity control ratio is more difficult, and all this is allly restricting the application of microcapsules in washing agent.For the microcapsules of coated essential oil, join in washing agent and mean and need to have stronger toughness and mechanical strength, the stability requirement of simultaneously storing is also higher.Therefore, need to be by melamine resin being carried out to modification to a certain degree to improve its mechanical performance and releasing properties.
Summary of the invention
In order to overcome the above-mentioned shortcoming and defect of prior art, the object of the present invention is to provide a kind of preparation method of urea modification melamine resin microcapsules of coated essential oil, the mechanical performances such as the toughness, fragility of melamine resin microcapsules have been improved, improve the compactness of microcapsules, extend the release time of essential oil, improved bin stability.
Object of the present invention is achieved through the following technical solutions:
A preparation method for the urea modification melamine resin microcapsules of coated essential oil, comprises the following steps:
(1) wall material precrosslink: take carbamide prepolymer as wall material, take urea as modifier, carry out precrosslink, obtain the wall material solution after precrosslink;
(2) core emulsification: take essential oil as core, form O/w emulsion with the wall material solution after precrosslink;
(3) cyst wall forms: stir O/w emulsion, form cyst wall;
(4) stop cross-linking reaction: add aqueous slkali to stop cross-linking reaction.
The described wall material of step (1) precrosslink: take carbamide prepolymer as wall material, take urea as modifier, carry out precrosslink, obtain the wall material solution after precrosslink, be specially:
In the dispersant of every 1.2 ~ 2.1g, add the deionized water of 120 ~ 160g, regulating pH is 8.0 ~ 9.0, under 30 ~ 50 ℃ of conditions, by dispersant emulsification 2h, is cooled to room temperature;
Add that 6.5 ~ 17.2g solid holdup is 24 ~ 50%, residual formaldehyde is lower than 0.2% carbamide prepolymer; Add formalin, making the formaldehyde total content adding is 0.18 ~ 0.32g; Add again the urea of 0.5 ~ 1.0g; Then with dilute solution of acetic acid, regulate pH=3.5 ~ 4.5, at ambient temperature, adjusting rotary speed 300 ~ 600rpm, stirs 105 ~ 150min; Described carbamide prepolymer with melamine and formaldehyde mass ratio in 1:(0.4 ~ 6) preparation.
The described core emulsification of step (2): take essential oil as core, form O/w emulsion with the wall material solution after precrosslink, be specially: the wall material solution after precrosslink is poured in emulsifying kettle, added 0.3 ~ 0.9g emulsifying agent, 0.2 ~ 0.6g defoamer, again regulating pH value is 3.5 ~ 4.5; Then, add the essential oil of 12.0 ~ 18.0g, in ice-water bath, regulate mulser rotating speed 1200 ~ 3000rpm, emulsification 30 ~ 40min, forms O/w emulsion.
The described cyst wall of step (3) forms: stir O/w emulsion, form cyst wall, be specially:
O/w emulsion is stirred to 30 ~ 40min with 300 ~ 600rpm speed at ambient temperature; Then, rising temperature to 65 ~ 75 ℃, stir 6 ~ 7h with 300 ~ 600rpm speed.
The described termination cross-linking reaction of step (4), adds aqueous slkali to stop cross-linking reaction, is specially:
The product that step (3) is obtained is cooled to room temperature, with sodium carbonate weak solution adjusting pH=10 ~ 11, stops cross-linking reaction.
The described dispersant of step (1) be in acrylic acid copolymer-maleic anhydride, styrene maleic anhydride copolymer and acrylamide-sodium acrylate copolymer any one or two or more.
The described emulsifying agent of step (2) be containing in the APES (OP-10) of 10 carbon atoms, Sorbitan ethoxylate (Tween-80), polyoxyethylene carboxylate any one or two or more.
The described defoamer of step (2) is arbitrary component in n-butanol, tributyl phosphate, water-based silicone oil or two or more.
The described emulsifying kettle of step (2) adopts 304# stainless steel to make, and internal diameter is 90mm, and wall thickness is 5mm, and emulsifying kettle inwall is welded with 3 baffle plates that are evenly distributed; The level cross-sectionn of described baffle plate is that central angle is 30 °, and what radius was 8mm is fan-shaped.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) to prepare microcapsule capsule wall material cheap and easy to get in the present invention, and preparation condition is easily realized, and reduced the cost of the coated essential oil microcapsules of preparation, is conducive to the large-scale production of this technology.
(2) emulsion process of the present invention adopts the stainless steel emulsifying kettle of autonomous Design, by adding three baffle plates, reduces widely whirlpool, increases the mutual collision frequency of drop.Meanwhile, added baffle plate, emulsification shearing force acts on drop more equably, and the emulsion droplet size distribution obtaining is also more even.
(3) the present invention adopts urea modification melamine resin to prepare microcapsules, has strengthened the toughness of microcapsules, has reduced fragility, has also improved the bin stability of microcapsules simultaneously, is conducive to the slow release of essential oil in microcapsules.
(4) the microcapsules residual formaldehyde that the strict amount that adds formaldehyde of controlling of the present invention, and monitoring prepares, the microcapsules residual formaldehyde preparing is lower than prescribed minimum.
(5) the urea modification melamine resin microcapsules of the coated essential oil that prepared by the present invention have good dispersiveness in aqueous solvent, are conducive to its application in washing agent.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the emulsifying kettle that adopts of embodiments of the invention 1.
Fig. 2 is the level cross-sectionn figure of Fig. 1.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
In 250mL round-bottomed flask, add 1.2g dispersant acrylic acid copolymer-maleic anhydride, the deionized water of 160g with 10% mass fraction NaOH solution adjusting pH=8.0, by dispersant emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the carbamide prepolymer that 17.2g solid holdup is 24%, residual formaldehyde is 0.19%; Add formalin, making the formaldehyde total content adding is 0.18g; Add again the urea of 0.84g; Then with dilute solution of acetic acid, regulate pH=4.5, at ambient temperature, adjusting rotary speed 300rpm, stirs 105min; Described carbamide prepolymer is prepared at 1:0.4 with melamine and formaldehyde mass ratio.Wall material solution after precrosslink is poured in emulsifying kettle, added 0.9g emulsifier op-10,0.6g defoamer n-butanol, again regulating pH value is 4.5.Then, add 18.0g essential oil, in ice-water bath, regulate mulser rotating speed 1200rpm, emulsification 30min, forms O/w emulsion.
The emulsion obtaining is poured in 250mL round-bottomed flask, under room temperature condition, with 300rpm speed, stirred 30min.Then, rising temperature to 65 ℃, stirs 6 hours with 300rpm speed.
The product that stirring was obtained after 6 hours is cooled to room temperature, with 10% mass fraction Na
2cO
3regulate pH=10, stop cross-linking reaction.
As shown in Figure 1 and 2, the emulsifying kettle that the present embodiment adopts is made by 304# stainless steel, and internal diameter is 90mm, and wall thickness is 5mm, and emulsifying kettle inwall is welded with 3 baffle plates 1 that are evenly distributed; The level cross-sectionn of described baffle plate 1 is that central angle is 30 °, and what radius was 8mm is fan-shaped.
For measuring residual formaldehyde in the urea modification melamine resin microcapsules of coated essential oil of preparation, adopt phenol reagent AAS (GB/18204.26-2000) to measure.
For measuring the average grain diameter of urea modification melamine resin microcapsules of coated essential oil of preparation, adopt the microcapsules that observation by light microscope makes also its size size distribution to be added up, obtain the average-size of microcapsules.
For measuring the encapsulation ratio of urea modification melamine resin microcapsules of coated essential oil of preparation, adopt thermogravimetric analysis roughly to determine the encapsulation ratio of microcapsules.
For measuring the roughly rate of release of urea modification melamine resin microcapsules of coated essential oil of preparation, in 30 ℃ of baking ovens, place 15 days after microcapsules are dry, weigh the weight change before and after placing, calculate residual mass percent.
Measurement result is as shown in table 1.
Embodiment 2
Embodiment 2 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
In 250mL round-bottomed flask, add 1.7g dispersant styrene maleic anhydride copolymer, the deionized water of 140g with 10%NaOH solution adjusting pH=8.0, by dispersant emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the carbamide prepolymer that 10g solid holdup is 36%, residual formaldehyde is 0.14%; Add formalin, making the formaldehyde total content adding is 0.26g; Add again the urea of 0.7g; Then with dilute solution of acetic acid, regulate pH=4.3, at ambient temperature, adjusting rotary speed 600rpm, stirs 150min; Described carbamide prepolymer is prepared at 1:2.5 with melamine and formaldehyde mass ratio.
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.4g emulsifier op-10,0.3g defoamer water-based silicone oil, again regulating pH value is 4.3.Then, add 15.0g essential oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min, forms O/w emulsion.
The emulsion obtaining is poured in 250mL round-bottomed flask, under room temperature condition, with 600rpm speed, stirred 40min.Then, rising temperature to 75 ℃, stirs 7 hours with 600rpm speed.
The product that stirring was obtained after 7 hours is cooled to room temperature, with 10% mass fraction Na
2cO
3regulate pH=11, stop cross-linking reaction.
Determination step is identical with embodiment 1, and measurement result is as shown in table 1.
Embodiment 3
Embodiment 3 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
In 250mL round-bottomed flask, add 2.1g acrylamide-sodium acrylate copolymer dispersant, the deionized water of 120g with 10% mass fraction NaOH solution adjusting pH=9.0, by dispersant emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the carbamide prepolymer that 6.5g solid holdup is 50%, residual formaldehyde is 0.15%; Add formalin, making the formaldehyde total content adding is 0.18g; Add again the urea of 0.5g; Then with dilute solution of acetic acid, regulate pH=3.5, at ambient temperature, adjusting rotary speed 500rpm, stirs 120min; Described carbamide prepolymer is prepared at 1:6 with melamine and formaldehyde mass ratio.
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.3g emulsifying agent Tween-80,0.2g defoamer n-butanol, again regulating pH value is 3.5.Then, add 12.0g essential oil, in ice-water bath, regulate mulser rotating speed 3000rpm, emulsification 40min, forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 4
Embodiment 4 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
Toward the mixture that adds 1.7g acrylic acid copolymer-maleic anhydride and acrylamide-sodium acrylate copolymer in 250mL round-bottomed flask, (wherein acrylic acid copolymer-maleic anhydride is 1g, acrylamide-sodium acrylate copolymer is 0.7g) as dispersant, the deionized water of 140g, with 10% mass fraction NaOH solution adjusting pH=8.0, under 50 ℃ of conditions, by dispersant emulsification 2h, be cooled to room temperature.Add the carbamide prepolymer that 7.2g solid holdup is 50%, residual formaldehyde is 0.2%; Add formalin, making the formaldehyde total content adding is 0.26g; Add again the urea of 0.9g; Then with dilute solution of acetic acid, regulate pH=4.5, at ambient temperature, adjusting rotary speed 300rpm, stirs 150min; Described carbamide prepolymer is prepared at 1:3 with melamine and formaldehyde mass ratio.
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.4g emulsifying agent polyoxyethylene carboxylate, 0.3g defoamer tributyl phosphate, again regulating pH value is 4.3.Then, add 15.0g essential oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min, forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 5
Embodiment 5 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.5g emulsifier op-10,0.4g defoamer n-butanol, again regulating pH value is 4.3.Then, add 15.0g essential oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min, forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 6
Embodiment 6 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
Toward the mixture that adds 1.9g styrene maleic anhydride copolymer, acrylic acid copolymer-maleic anhydride and acrylamide-sodium acrylate copolymer in 250mL round-bottomed flask, (wherein styrene maleic anhydride copolymer is 0.5g, acrylic acid copolymer-maleic anhydride is 1g, acrylamide-sodium acrylate copolymer is 0.4g) dispersant, the deionized water of 140g, with 10% mass fraction NaOH solution adjusting pH=8.0, under 50 ℃ of conditions, by dispersant emulsification 2h, be cooled to room temperature.Add the carbamide prepolymer that 7.2g solid holdup is 50%, residual formaldehyde is 0.2%; Add formalin, making the formaldehyde total content adding is 0.26g; Add again the urea of 0.7g; Then with dilute solution of acetic acid, regulate pH=4.5, at ambient temperature, adjusting rotary speed 600rpm, stirs 150min; Described carbamide prepolymer is prepared at 1:3 with melamine and formaldehyde mass ratio.
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.5g emulsifier op-10,0.4g defoamer n-butanol, again regulating pH value is 4.3.Then, add 15.0g essential oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min, forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
Embodiment 7
Embodiment 7 prepares the urea modification melamine resin microcapsules of coated essential oil according to the following steps:
In 250mL round-bottomed flask, add 1.7g acrylic acid copolymer-maleic anhydride dispersant, the deionized water of 140g with 10% mass fraction NaOH solution adjusting pH=8.0, by dispersant emulsification 2h, is cooled to room temperature under 50 ℃ of conditions.Add the carbamide prepolymer that 7.2g solid holdup is 50%, residual formaldehyde is 0.2%; Add formalin, making the formaldehyde total content adding is 0.26g; Add again the urea of 0.5 ~ 1.0g; Then with dilute solution of acetic acid, regulate pH=3.5, at ambient temperature, adjusting rotary speed 300rpm, stirs 150min; Described carbamide prepolymer is prepared at 1:3 with melamine and formaldehyde mass ratio.
Wall material solution after precrosslink is poured in emulsifying kettle, added 0.4g emulsifier op-10,0.3g defoamer n-butanol, again regulating pH value is 4.3.Then, add 15.0g essential oil, in ice-water bath, regulate mulser rotating speed 2000rpm, emulsification 30min, forms O/w emulsion.
Other preparation processes are identical with embodiment 1 with determination step, and measurement result is as shown in table 1.
The each embodiment location parameter of table 1
Above-described embodiment is preferably embodiment of the present invention, but embodiments of the present invention are not limited by the examples, if emulsifying agent can be the APES containing 10 carbon atoms, Sorbitan ethoxylate, two or more mixture in polyoxyethylene carboxylate, defoamer can be n-butanol, tributyl phosphate, two or more mixture in water-based silicone oil etc., other any do not deviate from the change of doing under Spirit Essence of the present invention and principle, modify, substitute, combination, simplify, all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. a preparation method for the urea modification melamine resin microcapsules of coated essential oil, is characterized in that, comprises the following steps:
(1) wall material precrosslink: take carbamide prepolymer as wall material, take urea as modifier, carry out precrosslink, obtain the wall material solution after precrosslink, be specially:
In the dispersant of every 1.2～2.1g, add the deionized water of 120～160g, regulating pH is 8.0～9.0, under 30～50 ℃ of conditions, by dispersant emulsification, is cooled to room temperature;
Add that 6.5～17.2g solid holdup is 24～50%, residual formaldehyde is lower than 0.2% carbamide prepolymer; Add formalin, making the formaldehyde total content adding is 0.18～0.32g; Add again the urea of 0.5～1.0g; Then with dilute solution of acetic acid, regulate pH=3.5～4.5, at ambient temperature, adjusting rotary speed 300～600rpm, stirs 105～150min; Described carbamide prepolymer with melamine and formaldehyde mass ratio in 1:(0.4～6) preparation;
(2) core emulsification: take essential oil as core, form O/w emulsion with the wall material solution after precrosslink, be specially: the wall material solution after precrosslink is poured in emulsifying kettle, added 0.3～0.9g emulsifying agent, 0.2～0.6g defoamer, again regulating pH value is 3.5～4.5; Then, add the essential oil of 12.0～18.0g, in ice-water bath, regulate mulser rotating speed 1200～3000rpm, emulsification 30～40min, forms O/w emulsion;
(3) cyst wall forms: stir O/w emulsion, form cyst wall:
O/w emulsion is stirred to 30～40min with 300～600rpm speed at ambient temperature; Then, rising temperature to 65～75 ℃, stir 6～7h with 300～600rpm speed;
(4) stop cross-linking reaction: add aqueous slkali to stop cross-linking reaction.
2. the preparation method of the urea modification melamine resin microcapsules of coated essential oil according to claim 1, is characterized in that, the described termination cross-linking reaction of step (4) adds aqueous slkali to stop cross-linking reaction, is specially:
The product that step (3) is obtained is cooled to room temperature, with sodium carbonate weak solution adjusting pH=10～11, stops cross-linking reaction.
3. the preparation method of the urea modification melamine resin microcapsules of coated essential oil according to claim 1, it is characterized in that, the described dispersant of step (1) be in acrylic acid copolymer-maleic anhydride, styrene maleic anhydride copolymer and acrylamide-sodium acrylate copolymer any one or two or more.
4. the preparation method of the urea modification melamine resin microcapsules of coated essential oil according to claim 1, it is characterized in that, the described emulsifying agent of step (2) be containing in the APES of 10 carbon atoms, Sorbitan ethoxylate, polyoxyethylene carboxylate any one or two or more.
5. the preparation method of the urea modification melamine resin microcapsules of coated essential oil according to claim 1, is characterized in that, the described defoamer of step (2) is arbitrary component in n-butanol, tributyl phosphate, water-based silicone oil or two or more.
6. the preparation method of the urea modification melamine resin microcapsules of coated essential oil according to claim 1, it is characterized in that, the described emulsifying kettle of step (2) adopts 304# stainless steel to make, and internal diameter is 90mm, wall thickness is 5mm, and emulsifying kettle inwall is welded with 3 baffle plates that are evenly distributed; The level cross-sectionn of described baffle plate is that central angle is 30 °, and what radius was 8mm is fan-shaped.
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| WO2017001672A1 (en) * | 2015-07-02 | 2017-01-05 | Givaudan Sa | Microcapsules |
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| CN113170920A (en) * | 2020-01-08 | 2021-07-27 | 中国科学院理化技术研究所 | Temperature-control heat-conducting multifunctional microcapsule for cigarettes and preparation method thereof |
| CN112841184A (en) * | 2021-01-28 | 2021-05-28 | 常州大学 | Physcion microcapsule sustained release agent and preparation method thereof |
| CN113999726B (en) * | 2021-08-18 | 2023-09-15 | 江苏集萃先进高分子材料研究所有限公司 | Essential oil microcapsule and preparation method thereof |
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