CN108704588A - A kind of preparation method of microencapsulation acidic aqueous solution - Google Patents
A kind of preparation method of microencapsulation acidic aqueous solution Download PDFInfo
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- CN108704588A CN108704588A CN201810693485.5A CN201810693485A CN108704588A CN 108704588 A CN108704588 A CN 108704588A CN 201810693485 A CN201810693485 A CN 201810693485A CN 108704588 A CN108704588 A CN 108704588A
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- aqueous solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
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Abstract
The invention discloses a kind of preparation methods of microencapsulation acidic aqueous solution comprising following steps：（1）Emulsifier and fatty acid methyl ester are uniformly mixed, acidic aqueous solution emulsion dispersion 10-30min is added under 500-5000 r/min stirring conditions, lotion is made；（2）Furfuryl alcohol and fatty acid methyl ester are uniformly mixed, are added to step under 400-800 r/min stirring conditions（1）Obtained lotion reacts 30-90min, and microcapsule suspensions are made；（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made.The microcapsules synthesis technology of the present invention is simple, and product controllability is strong, safety and environmental protection.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of preparation method of microencapsulation acidic aqueous solution.
Background technology
Microcapsules technology is a kind of protection technique encapsulated core material and to form fine particle, is slowly released with meeting it
It puts, abrupt release or the demand being persistently stored, is widely used in fields such as medicine, cosmetics, food, weaving and agriculturals.Especially
Being microencapsulation processing can make the mode of appearance of acidic aqueous solution become solid from liquid, come just for its storage and conveyer belt
Profit, and acidic aqueous solution, after microcapsule coated, stability improves, and can also realize slow release, is expected to be applied to catalysis
The fields such as agent, curing agent.For another example, phosphoric acid is a kind of excellent wood fire retardant, its water resistance can be improved after microcapsules processing,
Reduce its damage to strength of wood.
Core material involved in microcapsules is very extensive, according to the dissolubility of core material core material can be broadly divided into oil-soluble and
Water-soluble two major classes.Embedding core material realizes that the substance of micro-capsule gelatinization is known as wall material, and can be used as microcapsule wall material has natural polymer
Sub, semi-synthetic macromolecule and synthesis high molecular material.Wall material selection needs determined according to the property of core material, oil-soluble
Core material need to select water-soluble wall material, water-soluble core material then to select oil-soluble wall material, i.e. the solubility property of wall material and core material must not
Together, wall material cannot be reacted with core material, also not miscible with core material.In the prior art, water-soluble coating material type is more and holds
Easily obtain, and the oil-soluble coating material type that water-soluble core material is applicable in is few, and usually require to select in building-up process to have
The organic solvent of poison.Therefore, for water-soluble substances development technology, simple, safety and environmental protection microencapsulation technology has important meaning
Justice.
Furfuryl alcohol is to be made by furfural hydrogenation, and furfural is mainly derived from the crops such as bagasse, corncob and wheat stalk
The hydrolysis of by-product.Furfuryl alcohol polymerize under acidic catalyst effect obtained by thermosetting resin belong to environmentally friendly material, and have
There are good water resistance, heat resistance and resistance to acid and alkali, there is important use in fields such as binder, rubber and fibers.Develop base
In the microcapsules synthetic technology of furfuryl alcohol polycondensation reaction, is conducive to abundant microcapsules oil-soluble coating material type, promotes microcapsules
Environmentally protectiveization of product develops.
Fatty acid methyl ester is yellow clear liquid（It is colourless after rectifying）, there is a kind of mild, distinctive smell,
Stable structure, without corrosivity.Its also have relatively stronger solvability, volatile organic content is low, flash-point is high, nothing
It is malicious, biodegradable, it is a kind of environmentally friendly solvent.It, can be in the microcapsules synthetic technology based on furfuryl alcohol polycondensation reaction
Toxic organic solvents are substituted using Fatty acid methyl ester and dissolve furfuryl alcohol, develop the microencapsulation technology of safety and environmental protection.
Invention content
Against the above deficiency, the present invention provides a kind of preparation method of microencapsulation acidic aqueous solution, this method uses
Wall material raw material of the furfuryl alcohol as acidic aqueous solution microencapsulation, but using fatty acid methyl ester as solvent, under the action of catalyst, fat
Furfuryl alcohol in sour methyl esters gradually forms wall material in oil-water interfaces polymerization and wraps up acidic aqueous solution, and microcapsules are made.The microcapsules close
At simple for process, product controllability is strong, safety and environmental protection.
The present invention adopts the following technical scheme that realization：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）Emulsifier and fatty acid methyl ester are uniformly mixed, acidic aqueous solution is added under 500-5000 r/min stirring conditions
Lotion is made in emulsion dispersion 10-30min；
（2）Furfuryl alcohol and fatty acid methyl ester are uniformly mixed, are added to step under 400-800 r/min stirring conditions（1）It is made
The lotion obtained reacts 30-90min, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made.
Further, above-mentioned steps（1）In, the acidic aqueous solution is phosphoric acid, oxalic acid, sulfuric acid, hydrochloric acid and to toluene sulphur
Any one or a few mixed aqueous solutions in acid, sour mass fraction are 30%-85%.
Further, above-mentioned steps（1）In, the emulsifier is sorbitan fatty acid ester, specially span 20, department
Any one or a few mixing in disk 40, sorbester p18, sorbester p17 and span 85, emulsifier account for the mass fraction of fatty acid methyl ester
For 0.5%-3.5%, the volume ratio of fatty acid methyl ester and acidic aqueous solution is 4:1-8:1.
Further, above-mentioned steps（2）In, the mass fraction that furfuryl alcohol accounts for Fatty acid methyl ester in reaction system is 0.5%-8.0%.
Further, above-mentioned steps（2）In reaction temperature be 5-70 DEG C.
Further, above-mentioned steps（2）In, the volume ratio of the fatty acid methyl ester solution of lotion and furfuryl alcohol is 1:1-4:1.
Further, above-mentioned steps（3）In, centrifuging gained clear liquid can repeat as solvent to be used for step（1）And step
Suddenly（2）.
The technical program has the advantages that compared with prior art：
1, the method for the present invention disperses under emulsifier and mechanical agitation acidic aqueous solution to form core material drop；Then in liquid
In drop under sour catalytic action, the furfuryl alcohol in fatty acid methyl ester gradually forms the acid drop of wall material package in oil-water interfaces polymerization,
Microcapsules are made, it is simple for process, it is easy to operate.
2, the present invention uses wall material raw material of the furfuryl alcohol as acidic aqueous solution microencapsulation, because it in acid condition may be used
Wall material package core material drop is formed so that polymerisation occurs, without in addition catalyst of the addition for furfuryl alcohol polymerisation, favorably
In the cost that economizes on resources.
3, the fatty acid methyl ester that the present invention uses solvability strong, nontoxic, biodegradable is as in microencapsulation processes
The organic solvent of furfuryl alcohol improves the environmental safety of micro-encapsulation technology；Fatty acid methyl ester clear liquid after separation may be used also
It is reused using recycling as solvent, is conducive to save production cost.
4, the method for the present invention is simple for process, and product controllability is strong；Aliphatic acid when by adjusting emulsifier additive amount, emulsification
The volume ratio and emulsification rotating speed of methyl esters and acidic aqueous solution can effectively control the particle size of microcapsules, and by adjusting furfuryl alcohol
Mass fraction, reaction temperature and reaction time can effectively control the wall thickness and wall material compactness of microcapsules.
Specific implementation mode
Below with reference to embodiment, the invention will be further described, but not as limitation of the present invention.Following implementation
The specific experiment condition and method being not specified in example, used technological means are usually well-known to those skilled in the art normal
Rule means.
Embodiment 1：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.2g sorbester p17s and 14.6g Fatty acid methyl esters are uniformly mixed, 5.0g matter is added dropwise under 750 r/min stirring conditions
The phosphoric acid of score 85% is measured, lotion is made in emulsion dispersion 20min；
（2）1.0g furfuryl alcohols and 5.4g Fatty acid methyl esters are uniformly mixed, are slowly added to phosphoric acid under 500 r/min stirring conditions
Lotion reacts 60min at a temperature of 25 DEG C, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained phosphoric acid microcapsules are in regular spherical, favorable dispersibility, 2-11 μm of grain size.
Embodiment 2：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.3g sorbester p17s and 20.9g Fatty acid methyl esters are uniformly mixed, 7.1g matter is added dropwise under 750 r/min stirring conditions
The sulfuric acid of score 60% is measured, lotion is made in emulsion dispersion 10min；
（2）1.4g furfuryl alcohols and 7.7g Fatty acid methyl esters are uniformly mixed, are slowly added to sulfuric acid under 500 r/min stirring conditions
Lotion reacts 30min at a temperature of 25 DEG C, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained sulfuric acid microcapsules are in regular spherical, favorable dispersibility, 7-25 μm of grain size.
Embodiment 3：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.1g sorbester p17s, 0.1g span 20s and 15.0g Fatty acid methyl esters are uniformly mixed, in 2000 r/min stirring conditions
The lower mixed solution that 6.0g sulfuric acid and phosphoric acid is added dropwise, the sulfuric acid mass fraction 30% in the mixed solution, phosphoric acid quality score 30%,
Lotion is made in emulsion dispersion 10min；
（2）0.5g furfuryl alcohols and 10.0g Fatty acid methyl esters are uniformly mixed, are slowly added under 600 r/min stirring conditions to mixed
Yogurt liquid is closed, reacts 90min at a temperature of 60 DEG C, microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained sulfuric acid and phosphate mixture microcapsules are in regular spherical, favorable dispersibility, 1-10 μm of grain size.
Embodiment 4：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.075g span 85 and 15.0g Fatty acid methyl esters are uniformly mixed, 4.5g is added dropwise under 500 r/min stirring conditions
Lotion is made in the p-methyl benzenesulfonic acid of mass fraction 30%, emulsion dispersion 30min；
（2）1.3g furfuryl alcohols and 17.5g Fatty acid methyl esters are uniformly mixed, are slowly added to right under 400 r/min stirring conditions
Toluenesulfonic acid lotion reacts 60min at a temperature of 45 DEG C, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained p-methyl benzenesulfonic acid microcapsules are in regular spherical, favorable dispersibility, 10-35 μm of grain size.
Embodiment 5：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.7g span 40s and 20.0g Fatty acid methyl esters are uniformly mixed, 4.6g sulphur is added dropwise under 3000 r/min stirring conditions
The mixed solution of acid and hydrochloric acid, the sulfuric acid mass fraction 40% in the mixed solution, hydrochloric acid mass fraction 20%, emulsion dispersion
Lotion is made in 30min；
（2）2.1g furfuryl alcohols and 6.3g Fatty acid methyl esters are uniformly mixed, are slowly added to mixing under 800 r/min stirring conditions
Yogurt liquid reacts 90min at a temperature of 5 DEG C, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained sulfuric acid and hydrochloric acid mixture microcapsules are in regular spherical, favorable dispersibility, 1-5 μm of grain size.
Embodiment 6：
A kind of preparation method of microencapsulation acidic aqueous solution comprising following steps：
（1）0.2g sorbester p18s, 0.2g sorbester p17s and 15.0g Fatty acid methyl esters are uniformly mixed, in 5000 r/min stirring conditions
The lower mixed solution that 4.5g oxalic acid and p-methyl benzenesulfonic acid is added dropwise, the oxalic acid mass fraction 10% in the mixed solution, p-methyl benzenesulfonic acid
Lotion is made in mass fraction 30%, emulsion dispersion 30min；
（2）0.1g furfuryl alcohols and 5.0g Fatty acid methyl esters are uniformly mixed, are slowly added to mixing under 800 r/min stirring conditions
Yogurt liquid reacts 60min at a temperature of 70 DEG C, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made；From
The separating obtained clear liquid of the heart can repeat as solvent to be used for step（1）And step（2）.
Gained oxalic acid and p-methyl benzenesulfonic acid mixture microcapsules are in regular spherical, favorable dispersibility, 1-8 μm of grain size.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (7)
1. a kind of preparation method of microencapsulation acidic aqueous solution, it is characterised in that：It includes the following steps：
（1）Emulsifier and fatty acid methyl ester are uniformly mixed, acidic aqueous solution is added under 500-5000 r/min stirring conditions
Lotion is made in emulsion dispersion 10-30min；
（2）Furfuryl alcohol and fatty acid methyl ester are uniformly mixed, are added to step under 400-800 r/min stirring conditions（1）It is made
The lotion obtained reacts 30-90min, and microcapsule suspensions are made；
（3）By microcapsule suspensions after conventional centrifugation, washing and drying, powdered microcapsule product can be made.
2. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（1）In acidic aqueous solution be phosphoric acid, oxalic acid, sulfuric acid, hydrochloric acid and p-methyl benzenesulfonic acid in any one or a few mixing water
Solution, sour mass fraction are 30%-85%.
3. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（1）In, emulsifier is sorbitan fatty acid ester, specially in span 20, span 40, sorbester p18, sorbester p17 and span 85
Any one or a few mixing, the mass fraction that emulsifier accounts for fatty acid methyl ester is 0.5%-3.5%, fatty acid methyl ester with it is acid
The volume ratio of aqueous solution is 4:1-8:1.
4. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（2）In furfuryl alcohol account for Fatty acid methyl ester in reaction system mass fraction be 0.5%-8.0%.
5. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（2）In reaction temperature be 5-70 DEG C.
6. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（2）In, the volume ratio of the fatty acid methyl ester solution of lotion and furfuryl alcohol is 1:1-4:1.
7. a kind of preparation method of microencapsulation acidic aqueous solution according to claim 1, it is characterised in that：The step
（3）In, centrifuging gained clear liquid can repeat as solvent to be used for step（1）And step（2）.
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