CN109499347B - Slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres and preparation method thereof - Google Patents
Slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres and preparation method thereof Download PDFInfo
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- CN109499347B CN109499347B CN201811597079.5A CN201811597079A CN109499347B CN 109499347 B CN109499347 B CN 109499347B CN 201811597079 A CN201811597079 A CN 201811597079A CN 109499347 B CN109499347 B CN 109499347B
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Abstract
The invention provides a preparation method of a slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres, which comprises the following steps: dissolving sodium tripolyphosphate in distilled water to obtain sodium tripolyphosphate solution; dissolving tannin in distilled water to obtain water phase solution; dissolving ethyl cellulose and Tween-80 in toluene to obtain an oil phase solution; and mixing the water phase solution and the oil phase solution, stirring to form emulsion, adding a sodium tripolyphosphate solution for crosslinking, cooling, washing and drying to obtain the water-based emulsion. The invention also provides a slow-release formaldehyde trapping agent based on the ethyl cellulose tannin microspheres, which is prepared by the preparation method. The slow-release formaldehyde catching agent based on the ethyl cellulose tannin microspheres and the preparation method thereof are more environment-friendly, have good balling effect and are more beneficial to continuously catching formaldehyde.
Description
Technical Field
The invention relates to the technical field of formaldehyde trapping agents, in particular to a slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres and a preparation method thereof.
Background
Indoor air pollution has become a cause of various diseases, and formaldehyde is a main pollution source causing indoor air pollution. The main harm of formaldehyde is represented by stimulation to skin mucosa, and the indoor formaldehyde concentration is more than 0.08mg/m3It can cause many symptoms such as throat discomfort, chest distress, asthma, dermatitis, etc. At present, most of artificial boards are bonded by urea-formaldehyde resin adhesive, and the urea-formaldehyde resin adhesive is prepared by taking formaldehyde as a base material and can continuously release formaldehyde, so how to continuously capture and degrade the formaldehyde released in the artificial boards becomes a technical problem which needs to be solved in the technical field all the time.
The Chinese invention patent (application number 201310714723.3) discloses a microcapsule slow-release urea-formaldehyde resin formaldehyde catching agent and a preparation method thereof, wherein a core layer substance is one of urea, melamine and acrylamide, a shell layer material is one of methyl cellulose, ethyl cellulose and hydroxyethyl cellulose, and the preparation method comprises the following steps: 1) heating the liquid paraffin and the emulsifier under stirring until the liquid paraffin and the emulsifier are fully dissolved and uniformly mixed, and then cooling to room temperature, wherein the liquid paraffin and the emulsifier are a continuous phase; 2) uniformly stirring the solvent and the shell material in a water bath, then adding the core material, and stirring and dispersing to obtain a dispersion phase; 3) adding the dispersed phase into the continuous phase, stirring and dispersing for 10min, heating to 30-60 ℃, keeping the rotation speed at 800r/min for 5h, and cooling to room temperature; 4) filtering and washing the prepared microcapsule, and standing overnight under a vacuum condition to obtain the microcapsule slow-release urea-formaldehyde resin formaldehyde scavenger. The formaldehyde scavenger prepared by the preparation method takes urea, melamine and acrylamide as core layer substances, and the urea, the melamine and the acrylamide are chemical products, so that the formaldehyde scavenger is not beneficial to environmental protection. Moreover, the microcapsule prepared by the preparation method has an unstable structure, the shell material has poor coating property on core materials, the continuous capture of formaldehyde is not facilitated, and the balling effect needs to be further improved.
Disclosure of Invention
Problem (A)
In conclusion, the invention aims to provide a slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres and a preparation method thereof, so as to solve the technical problems that the preparation method of the formaldehyde trapping agent in the prior art is poor in balling effect and core layer materials are not environment-friendly.
(II) technical scheme
The first aspect of the embodiment of the invention provides a preparation method of a slow-release formaldehyde scavenger based on ethyl cellulose tannin microspheres, which comprises the following steps:
dissolving sodium tripolyphosphate in distilled water to obtain sodium tripolyphosphate solution;
dissolving tannin in distilled water to obtain water phase solution;
dissolving ethyl cellulose and Tween-80 in toluene to obtain an oil phase solution;
and mixing the water phase solution and the oil phase solution, stirring to form emulsion, adding the sodium tripolyphosphate solution for crosslinking, cooling, washing and drying to obtain the aqueous emulsion.
Optionally, the step of dissolving sodium tripolyphosphate in distilled water to obtain a sodium tripolyphosphate solution includes:
and correspondingly adding 1.2-1.4 mg of sodium tripolyphosphate into 1ml of distilled water, dissolving the sodium tripolyphosphate in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a sodium tripolyphosphate solution.
Optionally, the step of dissolving tannin in distilled water to obtain an aqueous solution comprises:
adding 1.5-2.5 mg of tannin into 2.5ml of distilled water correspondingly, dissolving the tannin in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a water phase solution.
Optionally, the step of dissolving ethyl cellulose and Tween-80 in toluene to prepare an oil phase solution comprises:
according to the proportion of correspondingly adding 15-25 mg of ethyl cellulose and 1.5-2.5 ml of Tween-80 into 100ml of toluene, dissolving the ethyl cellulose and the Tween-80 into the toluene, magnetically stirring at the rotating speed of 450-550 r/min for 30 minutes to obtain an oil phase solution.
Optionally, the step of mixing the water phase solution and the oil phase solution, stirring to form an emulsion, and adding the sodium tripolyphosphate solution for crosslinking includes:
stirring the oil phase solution, and dropwise adding the water phase solution while stirring according to the proportion that 22-28 ml of the water phase solution is correspondingly dropwise added into the oil phase solution containing 100ml of toluene;
stirring the mixture solution after the dropwise adding for 90-150 min at the rotating speed of 800-1400 r/min and the temperature of 40-60 ℃ so as to emulsify the mixture solution to form emulsion;
and adding a sodium tripolyphosphate solution into the emulsion, and continuously stirring at the rotating speed of 800-1400 r/min and the temperature of 40-60 ℃ for 90-150 min to crosslink the ethyl cellulose and the tannin.
Optionally, the step of dripping the mixture into the aqueous phase solution while stirring, wherein the stirring speed is 150-250 r/min.
Optionally, the steps of washing and drying after cooling comprise:
cooling the emulsified and crosslinked mixture solution to room temperature, washing the precipitate for 4-6 times by using acetone, and finally drying the product into powder in a drying oven at 55-65 ℃ to obtain the emulsified and crosslinked emulsion.
In a second aspect of the embodiment of the invention, the slow-release formaldehyde scavenger based on the ethyl cellulose tannin microspheres is provided, and is prepared according to the preparation method.
(III) technical effects
Compared with the prior art, the invention can achieve the following technical effects:
the formaldehyde catching agent prepared by the preparation method disclosed by the invention adopts the natural biomass material tannin as a core material, and is green, environment-friendly and renewable; in addition, the invention adopts toluene as an oil phase solvent, has better oil phase emulsifying effect and better balling effect; more importantly, the invention adopts an emulsion crosslinking method and sodium tripolyphosphate for crosslinking, and the crosslinking can form chemical bonds between molecules of the ethyl cellulose and the tannin, so that linear molecules are mutually connected to form a three-dimensional net structure, thus the sphere is more stable, the balling effect is better, and the tannin release time is longer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a microscopic picture of the sustained-release formaldehyde scavenger prepared by the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be described in more detail with reference to the following embodiments in order to make the technical aspects of the present invention more apparent and understandable.
Example 1
The embodiment of the invention provides a preparation method of a slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres, which comprises the following steps:
s101, dissolving sodium tripolyphosphate in distilled water to obtain a sodium tripolyphosphate solution.
S102, dissolving tannin in distilled water to prepare a water phase solution.
S103, dissolving ethyl cellulose and Tween-80 in toluene to prepare an oil phase solution.
And S104, mixing the water phase solution and the oil phase solution, stirring to form emulsion, adding a sodium tripolyphosphate solution for crosslinking, cooling, washing and drying to obtain the aqueous emulsion.
The preparation method of the formaldehyde scavenger provided by the embodiment of the invention takes tannin as a core material, and is green, environment-friendly and renewable; and sodium tripolyphosphate is adopted for crosslinking, toluene is used as an oil phase solvent, the balling effect is good, and the balling effect is shown in figure 1, wherein figure 1 is a microscopic picture of the slow-release formaldehyde scavenger prepared by the invention.
Example 2
The embodiment 2 of the invention is an embodiment of a preparation method of a slow-release formaldehyde trapping agent based on ethyl cellulose tannin microspheres, and the embodiment comprises the following steps:
s201, adding 1.2mg of sodium tripolyphosphate into 1ml of distilled water correspondingly, dissolving the sodium tripolyphosphate in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a sodium tripolyphosphate solution.
S202, correspondingly adding 1.5mg of tannin into 2.5ml of distilled water, dissolving the tannin into the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a water phase solution.
S203, adding 15mg of ethyl cellulose and 1.5ml of Tween-80 into 100ml of toluene correspondingly, dissolving the ethyl cellulose and the Tween-80 into the toluene, magnetically stirring at the rotating speed of 450r/min for 30 minutes to obtain an oil phase solution.
S204, stirring the oil phase solution, and according to the proportion that 22ml of water phase solution is correspondingly dripped into the oil phase solution containing 100ml of toluene, dripping the water phase solution while stirring, wherein the stirring speed is 150r/min (revolutions per minute).
S205, stirring the mixture solution after the dripping for 90min at the rotating speed of 800r/min and the temperature of 40 ℃ to emulsify the mixture solution to form emulsion.
S206, adding a sodium tripolyphosphate solution into the emulsion, and continuously stirring at the rotating speed of 800r/min and the temperature of 40 ℃ for 90min to enable the ethyl cellulose and the tannin to generate cross-linking.
S207, cooling the emulsified and crosslinked mixture solution to room temperature, washing the precipitate for 4 times by using acetone, and finally drying the product into powder at 60 ℃ in a drying oven.
Example 3
The embodiment 3 of the invention is another embodiment of a preparation method of a slow-release formaldehyde scavenger based on ethyl cellulose tannin microspheres, which comprises the following steps:
s301, adding 1.4mg of sodium tripolyphosphate into 1ml of distilled water correspondingly, dissolving the sodium tripolyphosphate in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a sodium tripolyphosphate solution.
S302, adding 2.5mg of tannin into 2.5ml of distilled water, dissolving the tannin into the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a water phase solution.
S303, correspondingly adding 25mg of ethyl cellulose and 2.5ml of Tween-80 according to the proportion of 100ml of toluene, dissolving the ethyl cellulose and the Tween-80 in the toluene, magnetically stirring at the rotation speed of 550r/min for 30 minutes to obtain an oil phase solution.
S304, stirring the oil phase solution, and according to the proportion that 28ml of water phase solution is correspondingly dripped into the oil phase solution containing 100ml of toluene, dripping the water phase solution while stirring, wherein the stirring speed is 250 r/min.
S305, stirring the mixture solution after the dripping at the rotation speed of 1400r/min and the temperature of 60 ℃ for 150min, and emulsifying the mixture solution to form emulsion.
S306, adding a sodium tripolyphosphate solution into the emulsion, and continuously stirring at the rotation speed of 1400r/min and the temperature of 60 ℃ for 150min to enable the ethyl cellulose and the tannin to generate cross-linking.
S307, cooling the emulsified and crosslinked mixture solution to room temperature, washing the precipitate for 6 times by using acetone, and finally drying the product into powder at 60 ℃ in a drying oven.
Example 4
The embodiment 4 of the invention is a preferable embodiment of a preparation method of a slow-release formaldehyde catching agent based on ethyl cellulose tannin microspheres, and the embodiment comprises the following steps:
s401, dissolving 13mg of sodium tripolyphosphate in 10ml of distilled water, stirring and dissolving until the solution is clear and transparent to obtain a sodium tripolyphosphate solution;
s402, preparing a water phase: 20mg of tannin is dissolved in 25ml of distilled water, and the mixture is stirred at room temperature and completely dissolved until the solution is clear and transparent.
S403, preparing an oil phase: 20mg of ethyl cellulose dry powder and 2ml of Tween-80 are dissolved in 100ml of toluene, and the mixture is magnetically stirred for 30 minutes at 500r/min to be uniformly dispersed.
S404, taking 100ml of toluene (containing 20mg of ethyl cellulose and 2ml of Tween-80) as an oil phase, dropwise adding 25ml of tannin solution (namely water phase solution) while stirring, and after dropwise adding, stirring the mixture at the rotating speed of 1100r/min for 120min at the temperature of 50 ℃ for emulsifying to form emulsion.
Preferably, the stirring speed when the aqueous phase solution is dripped is 200r/min, and the effect of better mixing the aqueous phase and the oil phase for the emulsification crosslinking reaction can be achieved by adopting the stirring speed.
Care should be taken to prevent the water phase from splashing and causing waste; the tannin is dripped at a fine flow rate, can be uniformly dripped at a rate of 100ml/min, and can not cause splashing.
S405, adding a sodium tripolyphosphate solution, keeping the temperature (50 ℃) and stirring (rotating speed 1100r/min) for 120 minutes, cooling to room temperature, washing the precipitate for 5 times by using acetone, and finally drying the product into powder in a 60-degree drying oven.
The sodium tripolyphosphate solution is added at one time without gradual dripping.
The acetone washing can dissolve and remove the residual toluene organic solvent in the precipitate.
The formaldehyde trapping agent prepared by the preparation method of the embodiment 4 has the best balling effect, and can release tannin more durably and stably so as to continuously trap formaldehyde.
Example 5
The embodiment of the invention also provides a slow-release formaldehyde trapping agent based on the ethyl cellulose tannin microspheres, which is prepared according to the preparation method of the embodiment 1-4.
Compared with the prior art, the slow-release formaldehyde trapping agent based on the ethyl cellulose tannin microspheres and the preparation method thereof provided by the embodiment of the invention have the following technical effects:
in the prior art, the microcapsule core material of the formaldehyde scavenger is acrylamide, melamine and urea which are chemical products, and the invention adopts natural biomass material tannin as the core material, so that the formaldehyde scavenger is green, environment-friendly and renewable;
the oil phase solvent adopted in the prior art is liquid paraffin, and the oil phase solvent adopted in the invention is toluene, so that the oil phase dissolving effect is better, and the balling effect is better;
the liquid phase drying method is adopted in the prior art, no crosslinking effect is performed, the emulsion crosslinking method is adopted, sodium tripolyphosphate is used for crosslinking, chemical bonds can be formed between molecules of ethyl cellulose and tannin through crosslinking, linear molecules are connected with each other to form a three-dimensional net structure, spheres are stable, and the tannin release time is longer.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (7)
1. The preparation method of the slow-release formaldehyde trapping agent based on the ethyl cellulose tannin microspheres is characterized by comprising the following steps:
dissolving sodium tripolyphosphate in distilled water to obtain sodium tripolyphosphate solution;
dissolving tannin in distilled water to obtain water phase solution;
dissolving ethyl cellulose and Tween-80 in toluene to obtain an oil phase solution;
stirring the oil phase solution, and dropwise adding the water phase solution while stirring according to the proportion that 22-28 ml of the water phase solution is correspondingly dropwise added into the oil phase solution containing 100ml of toluene;
stirring the mixture solution after the dropwise adding for 90-150 min at the rotating speed of 800-1400 r/min and the temperature of 40-60 ℃ so as to emulsify the mixture solution to form emulsion;
and adding the sodium tripolyphosphate solution into the emulsion, continuously stirring at the rotating speed of 800-1400 r/min and the temperature of 40-60 ℃ for 90-150 min to enable the ethyl cellulose and the tannin to be crosslinked, cooling, washing and drying to obtain the sodium tripolyphosphate emulsion.
2. The preparation method of the slow-release formaldehyde catching agent based on the ethylcellulose tannin microspheres as claimed in claim 1, wherein the step of dissolving sodium tripolyphosphate in distilled water to obtain a sodium tripolyphosphate solution comprises:
and correspondingly adding 1.2-1.4 mg of sodium tripolyphosphate into 1ml of distilled water, dissolving the sodium tripolyphosphate in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a sodium tripolyphosphate solution.
3. The method for preparing the slow-release formaldehyde catching agent based on the ethylcellulose tannin microspheres as claimed in claim 1, wherein the step of dissolving tannin in distilled water to obtain an aqueous solution comprises:
adding 1.5-2.5 mg of tannin into 2.5ml of distilled water correspondingly, dissolving the tannin in the distilled water, and stirring at room temperature until the solution is clear and transparent to obtain a water phase solution.
4. The preparation method of the slow-release formaldehyde catching agent based on the ethyl cellulose tannin microspheres as claimed in claim 1, wherein the step of dissolving ethyl cellulose and Tween-80 in toluene to prepare an oil phase solution comprises the following steps:
according to the proportion of correspondingly adding 15-25 mg of ethyl cellulose and 1.5-2.5 ml of Tween-80 into 100ml of toluene, dissolving the ethyl cellulose and the Tween-80 into the toluene, magnetically stirring at the rotating speed of 450-550 r/min for 30 minutes to obtain an oil phase solution.
5. The preparation method of the slow-release formaldehyde scavenger based on the ethylcellulose tannin microspheres as claimed in claim 1, wherein the step of dripping the formaldehyde scavenger into the aqueous phase solution while stirring at a speed of 150 to 250 r/min.
6. The preparation method of the slow-release formaldehyde scavenger based on the ethylcellulose tannin microspheres as claimed in claim 1, wherein the steps of washing and drying after cooling comprise:
cooling the emulsified and crosslinked mixture solution to room temperature, washing the precipitate for 4-6 times by using acetone, and finally drying the product into powder in a drying oven at 55-65 ℃ to obtain the emulsified and crosslinked emulsion.
7. The slow-release formaldehyde scavenger based on the ethyl cellulose tannin microspheres is characterized by being prepared according to the preparation method of any one of claims 1 to 6.
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CN102321488A (en) * | 2011-07-18 | 2012-01-18 | 中国科学技术大学 | A kind of derivatived cellulose micro-encapsulated halogen-free flame retardant and preparation method thereof |
CN103642069A (en) * | 2013-12-22 | 2014-03-19 | 北京化工大学 | Microcapsule controlled release-type urea resin formaldehyde catching agent and preparation method thereof |
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CN103642069A (en) * | 2013-12-22 | 2014-03-19 | 北京化工大学 | Microcapsule controlled release-type urea resin formaldehyde catching agent and preparation method thereof |
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