CN105753368A - Preparation method of jasminum essential oil sustained-release type functional decorative material - Google Patents
Preparation method of jasminum essential oil sustained-release type functional decorative material Download PDFInfo
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- CN105753368A CN105753368A CN201610066835.6A CN201610066835A CN105753368A CN 105753368 A CN105753368 A CN 105753368A CN 201610066835 A CN201610066835 A CN 201610066835A CN 105753368 A CN105753368 A CN 105753368A
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- quintessence oil
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
- B29C2043/5816—Measuring, controlling or regulating temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/58—Upholstery or cushions, e.g. vehicle upholstery or interior padding
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Structural Engineering (AREA)
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Abstract
The invention discloses a preparation method of a jasminum essential oil sustained-release type functional decorative material. The preparation method comprises the following series of technical means of adopting emulsified sodium alginate; jetting and extruding the emulsified sodium alginate through clearances, and solidifying into spherical shapes; performing freeze drying and vacuum freeze drying to form loose and porous microspheres; performing compound cross-linking, and effectively encapsulating jasminum essential oil, enabling the jasminum essential oil to be sufficiently stored inside the tiny loose and porous microspheres, and further enabling the jasminum essential oil to be uniformly dispersed inside a decorative material, and the like. By adopting the technical means, a final decorative material product can continuously and stably release fragrant flavor of the jasminum essential oil. In addition, the surfaces of the microspheres are coated with adhesive/emulsion, so that the air permeability of the microspheres is inhibited to a certain degree, and the sustained-release performance of the microspheres can be better maintained. The preparation method disclosed by the invention has the characteristics of low production cost, good sustained-release performance of the jasminum essential oil and the like. Products produced by the preparation method disclosed by the invention are suitable for high-grade interior decoration.
Description
Technical field
The preparation method that the present invention relates to a kind of functional ornamentation material, the preparation method particularly relating to a kind of jasmin quintessence oil spacetabs type functional ornamentation material；Belong to technical field of construction and decoration materials.
Background technology
Along with being rooted in the hearts of the people of growth in the living standard and environmental protection theory, people are more and more higher for the quality requirements of traditional building (decoration) material.Under the guide effect of the market demand, the research and development of functional building (decoration) material have become as a hot subject of those skilled in the art.Just because of this, in recent years, all kinds of buildings (decoration) material function is mined gradually, expands and extend, and Related product is introduced to the market in succession.
It is known that the jasmin quintessence oil extracted from Flos Jasmini Sambac, it is referred to as " king of quintessence oil ".Jasmin quintessence oil external application/smear and can nurse and improve scaly dry skin, hydropenia, excessively oily and sensitive situation, desalination striae gravidarum and cicatrix, increases skin elasticity, allows skin feel more tender.The fragrant gas that quintessence oil volatilization produces, it is a kind of to treat the active drug that severe psychiatric constrains, it is possible to consoles nerve, sets up a kind of self-confident, has optimistic and euphoria sensation, it is also possible to newborn and regain one's vigor.
Porcelain tendre is a kind of novel energy-saving low-carbon ornament materials of rising in recent years, and it is as decorative material for wall surface, has light weight, a feature such as flexible, appearance and modeling is various, good weatherability；It is used as floor decorative material, has the features such as wear-resisting, anti-skidding, comfortable foot feeling；Easy construction, quick, the ratio traditional material reduction of erection time, save space, save cost, and difficult drop-off.Suitable in building decorations such as exterior wall, interior wall, ground, it is particularly well-suited to the surface-veneer engineered of skyscraper exterior finish engineering, facade decorative engineering, exterior wall plane materiel, the finish coat of external insulation system and the opposite sex building such as curved wall, arch post.Particularly, when porcelain tendre is for inner-outer wall renovation construction, old basal plane need not be knocked out.Thus, quick construction is easy, quantities is little and without building waste output.Particularly porcelain tendre also has the feature of good permeability.
Assume the jasmin quintessence oil " cladding " of purification by liquid extraction from natural plants in the ornament materials of indoor decoration, in conjunction with the feature of porcelain tendre good permeability, so that jasmin quintessence oil sustained release, become the functional ornamentation material with the market competitiveness by being expected to.
But, how to develop good with the ornament materials compatibility, can effectively " solidification " inside ornament materials, to carry the carrier of carrying liquid jasmin quintessence oil, and how effectively to control volatilization or the rate of release of jasmin quintessence oil, become those skilled in the art and carry out such research and development of products, it is necessary to first solve the technical problem that.
Summary of the invention
It is an object of the present invention to provide the preparation method that a kind of sustained release performance is good, can discharge the jasmin quintessence oil spacetabs type functional ornamentation material of jasmin quintessence oil fragrance sustainedly and stably.
The present invention be employed technical scheme comprise that for achieving the above object, the preparation method of a kind of jasmin quintessence oil spacetabs type functional ornamentation material, it is characterised in that comprise the following steps:
The first step, prepared by jasmin quintessence oil microsphere:
In mass ratio 155 15, weigh jasmin quintessence oil, polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium alginate respectively, standby；
By taken jasmin quintessence oil, polyoxyethylene sorbitan trioleate and glycerol monostearate, mixing, newborn even 5min, prepare the first mixed emulsion；
And taken sodium alginate is configured to the sodium alginate soln that mass percent concentration is 3-5%；
Then, above-mentioned first mixed emulsion is joined in the sodium alginate soln that mass percent concentration is 3-5%, stir 30min, obtain sodium alginate emulsion；
Obtained sodium alginate emulsion is entered fluid reservoir, then, adopts gap spray regime, be the CaCl of 4-5% through the first orifice plate injection to mass percent concentration by sodium alginate emulsion2In solution, so that sodium alginate emulsion is at CaCl2Solution is frozen into spherical；In course of injection, continuously stirred CaCl2Solution；
The aperture of above-mentioned first orifice plate is 3mm；
Described gap spray regime refers to that speed is 1 time/5 seconds, and the interval time between adjacent twice injection is 5 seconds；
After whole sodium alginate emulsions extrusion solidification forming, first centrifugation, after solid content is respectively washed 1 time with acetone, ethanol, distilled water successively；
Then, then by solid content vacuum lyophilization 1-3 hour at-20 DEG C after washing, prepare and make dry microsphere at the beginning of jasmin quintessence oil；
Second step, prepared by composite crosslinked microsphere:
Being immersed in jasmin quintessence oil by microsphere processed at the beginning of gained jasmin quintessence oil, absorb to saturation until microsphere processed at the beginning of jasmin quintessence oil, leaching goes out, and obtains the wet microsphere of jasmin quintessence oil, standby；
3rd step, 1:1:10 in mass ratio, take polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium carboxymethyl cellulose respectively, and sodium carboxymethyl cellulose is added distilled water, be configured to the carboxymethylcellulose sodium solution that mass percent concentration is 10-15%；
By taken polyoxyethylene sorbitan trioleate and glycerol monostearate, it is added separately in above-mentioned carboxymethylcellulose sodium solution, after newborn even 15min, prepares the second mixed emulsion；
4th step, is immersed in above-mentioned second mixed emulsion by wet for above-mentioned jasmin quintessence oil microsphere, and mix and blend 30min, to form uniform suspended emulsion；
Then, above-mentioned suspended emulsion being entered fluid reservoir, adopt above-mentioned gap spray regime, via hole diameter is second orifice plate of 6mm, by suspended emulsion injection to mass percent concentration be in 15-18% aluminum potassium sulfate solution；In course of injection, continuously stirred aluminum potassium sulfate solution；
After fully reaction, centrifugation, after respectively wash 1 time with normal hexane, ethanol, distilled water successively, obtain composite crosslinked microsphere after lyophilization；
5th step, the molding of ornament materials:
By mass fraction, take the macromolecular elastomer of 100-160 part respectively, 400-500 part inorganic filler, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 80-100 part composite crosslinked microsphere, after being uniformly mixed,
Join in mould, compressing at 150-180 DEG C, and emboss 5-10min at 180-200 DEG C；After heat preservation solidification 1-2h, the demoulding；And it is cooled to room temperature with the rate of temperature fall of 3-10 DEG C/min, to obtain final product.
Being preferably, above-mentioned macromolecular elastomer is one or more in polyacrylate, ethylene-vinyl acetate copolymer or polyurethane.
It is preferred that, above-mentioned inorganic filler be the cement block after grinding, ceramics or marmorean one or more, the particle diameter after grinding is 20-50 μm.
It is preferred that, the chemical composition of above-mentioned adhesive is neoprene latex.
It is preferred that, above-mentioned jasmin quintessence oil all extracts as follows:
The first step, the jasmine after super-dry of learning from else's experience, enter pulverizer and be ground into graininess, standby；
Second step, the in mass ratio ratio of 1:25, by granular jasmine submergence in organic solvent, enter annular rotary funace, at 150 DEG C, and rotary heating 24h；
Then, filter 23-5 times, take filtering residue, under 110 DEG C of conditions, carry out decompression distillation, to remove remaining organic solvent, obtain jasmin quintessence oil crude product；
3rd step, adopts silicagel column separate mode, the thick product of quintessence oil is purified, to obtain final product；
Above-mentioned organic solvent is petroleum ether, normal hexane, ethyl acetate, one or more in acetone.
What technique scheme was directly brought has the technical effect that, adopt the sodium alginate through Over emulsfication, through gap injection extrusion, be frozen into spherical, and it is freeze-dried and after vacuum lyophilization, form " microsphere " of loose porous shape, then through composite crosslinking, jasmin quintessence oil to be formed effective encapsulating so that jasmin quintessence oil fully " storage " is internal at " microsphere " of tiny loose porous shape, and then the series technique means such as the inside being dispersed in ornament materials
Make final ornament materials product can continue, stably slowly release jasmin quintessence oil fragrance.Further, due to, above-mentioned " microsphere " surface is by glue/breast cladding, and its breathability is inhibited to a certain extent, it is possible to keep its sustained release performance preferably.
In technique scheme, the microsphere storing jasmin quintessence oil passes through composite crosslinking, and its rich surface, containing substantial amounts of polar group, is beneficial between itself and ornament materials and forms bonding action, form an organic whole.It is to say, the introducing of " microsphere ", not only it is not result in the physical properties index of final products ornament materials, and, this " microsphere " carrying a large amount of jasmin quintessence oil composition is dispersed in final obtained ornament materials.
In technique scheme, making dry microsphere at the beginning of jasmin quintessence oil is that vacuum lyophilization shapes under the low temperature of-20 degree, on the one hand, the physical arrangement change of its material is less, and its organizational structure is preserved preferably；More it is essential that after microsphere lyophilization, its internal spongy in porous, save more inner space, thus there is the absorbability of excellence, adsorbable essential oil droplets is until saturated.
In technique scheme, why selecting sodium alginate to prepare raw material as jasmin quintessence oil " carrier ", reason is in that, sodium alginate is a kind of anionic polyelectrolyte polysaccharide, utilizes calcium ion crosslinking can form gel micro-ball.And the microsphere formed can be coated with quintessence oil molecule so that it is not easily leak；
Meanwhile, adopting lyophilization mode, sodium alginate calcium surface is porous spongy, improves the absorbability of material, contributes to the absorption again of quintessence oil.
Further, the introducing of follow-up sodium carboxymethyl cellulose, it is mainly in view of, carboxyl and Al in the molecular structure of sodium carboxymethyl cellulose3+Coordination forms micro-crosslinking, quintessence oil can be implemented effectively encapsulating and the firm molding of microsphere, after composite crosslinking, be beneficial to the slow release of jasmin quintessence oil molecule.
In technique scheme, primary raw material wide material sources, cheap, pollution-free in whole production process, discharge without venomous injurant.
Additionally, in technique scheme, what the extracting of jasmin quintessence oil adopted is solvent extraction method, and simply, easily operate, productivity is high, cost is low for its processing step.
In sum, the present invention, relative to prior art, has production cost sustained release performance low, jasmin quintessence oil good.That is, functional, the stability of ornament materials product and the beneficial effect such as reliability is good.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Illustrate: following embodiment, the jasmin quintessence oil used, all extract as follows:
The first step, the Flos Jasmini Sambac after super-dry of learning from else's experience, enter pulverizer and be ground into graininess, standby；
Second step, the in mass ratio ratio of 1:25, by granular Flos Jasmini Sambac submergence in organic solvent, enter annular rotary funace, at 150 DEG C, and rotary heating 24h；
Then, filter 23-5 times, take filtering residue, under 110 DEG C of conditions, carry out decompression distillation, to remove remaining organic solvent, obtain jasmin quintessence oil crude product；
3rd step, adopts silicagel column separate mode, the thick product of quintessence oil is purified, to obtain final product；
Above-mentioned organic solvent is petroleum ether, normal hexane, ethyl acetate, one or more in acetone.
The preparation method of embodiment 1 jasmin quintessence oil spacetabs type functional ornamentation material comprises the following steps:
The first step, prepared by jasmin quintessence oil microsphere:
In mass ratio 155 15, weigh jasmin quintessence oil, polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium alginate respectively, standby；
By taken jasmin quintessence oil, polyoxyethylene sorbitan trioleate and glycerol monostearate, mixing, newborn even 5min, prepare the first mixed emulsion；
And taken sodium alginate is configured to the sodium alginate soln that mass percent concentration is 3-5%；
Then, above-mentioned first mixed emulsion is joined in the sodium alginate soln that mass percent concentration is 3-5%, stir 30min, obtain sodium alginate emulsion；
Obtained sodium alginate emulsion is entered fluid reservoir, then, adopts gap spray regime, be the CaCl of 4-5% through the first orifice plate injection to mass percent concentration by sodium alginate emulsion2In solution, so that sodium alginate emulsion is at CaCl2Solution is frozen into spherical；In course of injection, continuously stirred CaCl2Solution；
The aperture of above-mentioned first orifice plate is 3mm；
Above-mentioned gap spray regime refers to that speed is 1 time/5 seconds, and the interval time between adjacent twice injection is 5 seconds；
After whole sodium alginate emulsions extrusion solidification forming, first centrifugation, after solid content is respectively washed 1 time with acetone, ethanol, distilled water successively；
Then, then by solid content vacuum lyophilization 3 hours at-20 DEG C after washing, prepare and make dry microsphere at the beginning of jasmin quintessence oil；
Second step, prepared by composite crosslinked microsphere:
Being immersed in jasmin quintessence oil by microsphere processed at the beginning of gained jasmin quintessence oil, absorb to saturation until microsphere processed at the beginning of jasmin quintessence oil, leaching goes out, and obtains the wet microsphere of jasmin quintessence oil, standby；
3rd step, 1:1:10 in mass ratio, take polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium carboxymethyl cellulose respectively, and sodium carboxymethyl cellulose is added distilled water, be configured to the carboxymethylcellulose sodium solution that mass percent concentration is 10-15%；
By taken polyoxyethylene sorbitan trioleate and glycerol monostearate, it is added separately in above-mentioned carboxymethylcellulose sodium solution, after newborn even 15min, prepares the second mixed emulsion；
4th step, is immersed in above-mentioned second mixed emulsion by wet for above-mentioned jasmin quintessence oil microsphere, and mix and blend 30min, to form uniform suspended emulsion；
Then, above-mentioned suspended emulsion being entered fluid reservoir, adopt above-mentioned gap spray regime, via hole diameter is second orifice plate of 6mm, by suspended emulsion injection to mass percent concentration be in 15-18% aluminum potassium sulfate solution；In course of injection, continuously stirred aluminum potassium sulfate solution；
After fully reaction, centrifugation, after respectively wash 1 time with normal hexane, ethanol, distilled water successively, obtain composite crosslinked microsphere after lyophilization；
5th step, the molding of ornament materials:
By mass fraction, take the macromolecular elastomer of 100 parts respectively, 400 parts of inorganic fillers, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 80 parts of composite crosslinked microspheres, after being uniformly mixed, join in mould, at 150-180 DEG C compressing, and 180-200 DEG C emboss 5-10min；After heat preservation solidification 1-2h, the demoulding；And it is cooled to room temperature with the rate of temperature fall of 3-10 DEG C/min, to obtain final product.
Above-mentioned macromolecular elastomer is polyacrylate.
Above-mentioned inorganic filler is the cement block after grinding, ceramics or marmorean mixture, and the diameter of particle after grinding is 20-50 μm.The chemical composition of above-mentioned adhesive is neoprene latex.
Embodiment 2
Except " by mass fraction, take the macromolecular elastomer of 120 parts respectively, 450 parts of inorganic fillers, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 90 parts of composite crosslinked microspheres ", macromolecular elastomer are outside ethylene-vinyl acetate copolymer；All the other, all with embodiment 1.
Embodiment 3
Except being polyurethane except macromolecular elastomer；All the other, all with embodiment 1.
Embodiment 4
" by mass fraction, take the macromolecular elastomer of 160 parts respectively, 450 parts of inorganic fillers, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 100 parts of composite crosslinked microspheres " outward；All the other, all with embodiment 1.
Embodiment 5
" by mass fraction, take the macromolecular elastomer of 145 parts respectively, 500 parts of inorganic fillers, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 100 parts of composite crosslinked microspheres " outward；All the other, all with embodiment 1.
The detection of product and inspection:
1, the functional detection of jasmin quintessence oil slow-releasing.
Method is as follows: the interior wall in 5 different rooms is carried out interior decoration by the functional ornamentation material product obtained by Example 1-5 respectively, and windows through hold-open door, to keep indoor air flows smooth and easy.
Use gas detector, carry out an indoor air quality monitoring week about, continue 50 weeks.Monitoring result shows: gas concentration is not any change.
In each indoor air quality monitoring process, select 1-2 people in company with entering room, and deeply breathe, all can feel the light jasmine fragrance having one " like without seemingly having ", feel very comfortable.
Illustrate: the jasmin quintessence oil fragrance concentration that product discharges is very low, and sustained release performance is good.
2, ornament materials physical property detection contrast
By functional ornamentation material product obtained by embodiment 1-5 with that produce according to a conventional method, have composite crosslinked microsphere except undoped p except, the ornament materials product contrast that other each raw materials are identical with the raw materials used kind of embodiment 1-5 and proportioning respectively.
Comparing result is table 1 below such as:
| Index | Water absorption rate | Tearing strength kN/m | Hot strength MPa | Stain resistance | Pliability |
| Embodiment 1 | 1.6% | 25 | 6.5 | 4 grades | Good |
| Contrast sample 1 | 1.58% | 23.5 | 6.4 | 4 grades | Good |
| Embodiment 2 | 1.55% | 25 | 6.1 | 4 grades | Good |
| Contrast sample 2 | 1.5% | 24 | 5.9 | 4 grades | Good |
| Embodiment 3 | 1.65% | 25 | 6.2 | 4 grades | Good |
| Contrast sample 3 | 1.58% | 24 | 6.0 | 4 grades | Good |
| Embodiment 4 | 1.5% | 24 | 6.4 | 4 grades | Good |
| Contrast sample 4 | 1.5% | 23.5 | 6.2 | 4 grades | Good |
| Embodiment 5 | 1.45% | 25 | 5.8 | 4 grades | Good |
| Contrast sample 5 | 1.43% | 24.5 | 5.88 | 4 grades | Good |
Comparing result shows: the introducing of composite crosslinked microsphere, on the Main physical performance indications of ornament materials almost without any impact.Get rid of detection error component, it can be seen that on the contrary, in water absorption rate, hot strength and tearing toughness etc., even also create trickle improvement result.
Claims (5)
1. the preparation method of a jasmin quintessence oil spacetabs type functional ornamentation material, it is characterised in that comprise the following steps:
The first step, prepared by jasmin quintessence oil microsphere:
In mass ratio 155 15, weigh jasmin quintessence oil, polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium alginate respectively, standby；
By taken jasmin quintessence oil, polyoxyethylene sorbitan trioleate and glycerol monostearate, mixing, newborn even 5min, prepare the first mixed emulsion；
And taken sodium alginate is configured to the sodium alginate soln that mass percent concentration is 3-5%；
Then, above-mentioned first mixed emulsion is joined in the sodium alginate soln that mass percent concentration is 3-5%, stir 30min, obtain sodium alginate emulsion；
Obtained sodium alginate emulsion is entered fluid reservoir, then, adopts gap spray regime, be the CaCl of 4-5% through the first orifice plate injection to mass percent concentration by sodium alginate emulsion2In solution, so that sodium alginate emulsion is at CaCl2Solution is frozen into spherical；In course of injection, continuously stirred CaCl2Solution；
The aperture of above-mentioned first orifice plate is 3mm；
Described gap spray regime refers to that speed is 1 time/5 seconds, and the interval time between adjacent twice injection is 5 seconds；
After whole sodium alginate emulsions extrusion solidification forming, first centrifugation, after solid content is respectively washed 1 time with acetone, ethanol, distilled water successively；
Then, then by solid content vacuum lyophilization 1-3 hour at-20 DEG C after washing, prepare and make dry microsphere at the beginning of jasmin quintessence oil；
Second step, prepared by composite crosslinked microsphere:
Being immersed in jasmin quintessence oil by microsphere processed at the beginning of gained jasmin quintessence oil, absorb to saturation until microsphere processed at the beginning of jasmin quintessence oil, leaching goes out, and obtains the wet microsphere of jasmin quintessence oil, standby；
3rd step, 1:1:10 in mass ratio, take polyoxyethylene sorbitan trioleate, glycerol monostearate and sodium carboxymethyl cellulose respectively, and sodium carboxymethyl cellulose is added distilled water, be configured to the carboxymethylcellulose sodium solution that mass percent concentration is 10-15%；
By taken polyoxyethylene sorbitan trioleate and glycerol monostearate, it is added separately in above-mentioned carboxymethylcellulose sodium solution, after newborn even 15min, prepares the second mixed emulsion；
4th step, is immersed in above-mentioned second mixed emulsion by wet for above-mentioned jasmin quintessence oil microsphere, and mix and blend 30min, to form uniform suspended emulsion；
Then, above-mentioned suspended emulsion being entered fluid reservoir, adopt above-mentioned gap spray regime, via hole diameter is second orifice plate of 6mm, by suspended emulsion injection to mass percent concentration be in 15-18% aluminum potassium sulfate solution；In course of injection, continuously stirred aluminum potassium sulfate solution；
After fully reaction, centrifugation, after respectively wash 1 time with normal hexane, ethanol, distilled water successively, obtain composite crosslinked microsphere after lyophilization；
5th step, the molding of ornament materials:
By mass fraction, take the macromolecular elastomer of 100-160 part respectively, 400-500 part inorganic filler, 3-6 part foaming agent, 3-6 part dispersant, 10-40 part adhesive, 80-100 part composite crosslinked microsphere, after being uniformly mixed,
Join in mould, compressing at 150-180 DEG C, and emboss 5-10min at 180-200 DEG C；After heat preservation solidification 1-2h, the demoulding；And it is cooled to room temperature with the rate of temperature fall of 3-10 DEG C/min, to obtain final product.
2. the preparation method of jasmin quintessence oil spacetabs type functional ornamentation material according to claim 1, it is characterised in that described macromolecular elastomer is one or more in polyacrylate, ethylene-vinyl acetate copolymer or polyurethane.
3. the preparation method of jasmin quintessence oil spacetabs type functional ornamentation material according to claim 1, it is characterised in that described inorganic filler be the cement block after grinding, ceramics or marmorean one or more, the particle diameter after grinding is 20-50 μm.
4. the preparation method of jasmin quintessence oil spacetabs type functional ornamentation material according to claim 1, it is characterised in that the chemical composition of described adhesive is neoprene latex.
5. the preparation method according to the arbitrary described jasmin quintessence oil spacetabs type functional ornamentation material of claim 1-4, it is characterised in that described jasmin quintessence oil extracts as follows:
The first step, the Flos Jasmini Sambac after super-dry of learning from else's experience, enter pulverizer and be ground into graininess, standby；
Second step, the in mass ratio ratio of 1:25, by granular Flos Jasmini Sambac submergence in organic solvent, enter annular rotary funace, at 150 DEG C, and rotary heating 24h；
Then, filter 23-5 times, take filtering residue, under 110 DEG C of conditions, carry out decompression distillation, to remove remaining organic solvent, obtain jasmin quintessence oil crude product；
3rd step, adopts silicagel column separate mode, the thick product of quintessence oil is purified, to obtain final product；
Above-mentioned organic solvent is petroleum ether, normal hexane, ethyl acetate, one or more in acetone.
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| CN201610066835.6A CN105753368B (en) | 2016-02-01 | 2016-02-01 | A kind of preparation method of refined jasmine oil spacetabs type functional ornamentation material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10363205B2 (en) | 2016-10-26 | 2019-07-30 | Elc Management Llc | Delayed release delivery systems and methods |
| US10661244B2 (en) | 2016-10-26 | 2020-05-26 | Elc Management Llc | Delayed release delivery systems and methods |
| CN111316952A (en) * | 2020-03-18 | 2020-06-23 | 暨南大学 | Sustained-release oxygen-increasing granule and preparation method and application thereof |
| CN114016161A (en) * | 2021-12-03 | 2022-02-08 | 西南大学 | Alginate gel fiber and preparation method thereof |
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| CN1396200A (en) * | 2002-06-08 | 2003-02-12 | 福建省泉州正亿实业有限公司 | Composition used to make shoe sole |
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| CN1396200A (en) * | 2002-06-08 | 2003-02-12 | 福建省泉州正亿实业有限公司 | Composition used to make shoe sole |
| CN101649254A (en) * | 2009-09-14 | 2010-02-17 | 太仓文华实业有限公司 | Micro-capsule essence with two-layer capsule wall and preparation method and application thereof |
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Cited By (4)
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| US10363205B2 (en) | 2016-10-26 | 2019-07-30 | Elc Management Llc | Delayed release delivery systems and methods |
| US10661244B2 (en) | 2016-10-26 | 2020-05-26 | Elc Management Llc | Delayed release delivery systems and methods |
| CN111316952A (en) * | 2020-03-18 | 2020-06-23 | 暨南大学 | Sustained-release oxygen-increasing granule and preparation method and application thereof |
| CN114016161A (en) * | 2021-12-03 | 2022-02-08 | 西南大学 | Alginate gel fiber and preparation method thereof |
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| CN105753368B (en) | 2018-02-06 |
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