CN107714534A - A kind of preparation method of the microcapsules with antipollution effect - Google Patents

Abstract

The present invention relates to a kind of preparation method of the microcapsules with antipollution effect, it is characterised in that using following steps：A, gelatin, Arabic gum, distilled water are weighed in mass ratio, prepare aqueous gelatin solution and the Arabic gum aqueous solution respectively；B, in mass ratio 2 ~ 6:3~8:3~5:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract and brown algae polyphenols, and antipollution active compound is used as after mixing；25 ~ 55^oUnder C water bath conditions, mixed with the Arabic gum aqueous solution, add yeast extract ultrasonic emulsification, then add aqueous gelatin solution, finally add acetum regulation system pH, room temperature is cooled to after aggregation；C, 5 ~ 10 are subsequently placed in^oIn C cold baths, add formalin and carry out crosslinking curing, stand to obtain microcapsules sedimentation liquid；D, microcapsules sedimentation liquid is filtered, washed, dried, produce the microcapsules with antipollution effect.The present invention has the advantages that stability is good, conveniently added, can help skin resistance varying environment pollution infringement.

Description

A kind of preparation method of the microcapsules with antipollution effect

Technical field

The invention belongs to technical field of cosmetic preparation, more particularly to a kind of preparation of the microcapsules with antipollution effect Method.

Technical background

With the continuous development of Global Urbanization process, people's living environment is also destroyed therewith：Coal-fired and car tail Gas brings PM2.5 particulates；The a large amount of of the chemical substances such as fluorochloroparaffins use the ozone decomposed caused in stratosphere, so as to get up to ground The uitraviolet intensity enhancing in face；The effect of oxynitrides and hydrocarbon in vehicle exhaust, industrial waste gas in ultraviolet light Third contact of a total solar or lunar eclipse chemical reaction is issued, generates ozone（O₃）, acetylperoxide（PAN）Deng secondary pollution, it is mixed to form with primary pollution Photochemical fog.Above-mentioned pollution factor not in the skin of infringement people, causes pachylosis, sensitivity, cuticula to become all the time Thickness is hardened, aging, the unequal skin problem of the colour of skin.

At present, generally believe that environmental pollution mainly damages in terms of following three to skin：1）Suspend in atmosphere Fine particle（Such as PM 2.5）, specific surface area is big, has tiny loose structure, easily absorption such as polycyclic aromatic hydrocarbon（PAHs）, nitrogen oxygen The poisonous and harmful substances such as compound, heavy metal, microorganism.This kind of particulate matter easily attaches to lipophilic skin surface, constantly release Its poisonous and harmful substance adsorbed, these small-molecule substances, into skin depths, be able to can not only be broken by the use of pore as passage Bad skin health cell, induce inflammation, can also influence the gene expression related to skin barrier function and skin texture function, So as to weaken the barrier function of skin, cause skin increasingly sensitive, and trigger the obscure, color spot of premature aging, the colour of skin etc. a series of Skin problem；2）Photochemical pollution takes place frequently, and is used plus the high frequency of indoor printer, duplicator, disinfection cabinet, can allow skin Skin is often exposed in O3 environment, and O3 strong oxidizing property can destroy skin surface lipid barrier, and induced activity oxygen cluster（ROS）It is raw Into, cellular damage is caused, or even the structure of skin corium collagen and elastin laminin can be destroyed, cause skin to wrinkle too early Line；3）The appearance of ozone hole causes uitraviolet intensity increase in earth's surface, and ultraviolet can cause intracellular DNA, mitochondria damage Wound, causes skin barrier function to be damaged, the degraded of collagen, elastin laminin and hyaluronic acid, makes dry skin sensitive, loses Elasticity, there is microgroove.

In summary, environmental pollution is that skin is caused to encroach on from many aspects, wants to reduce and repair with skin care item Multiple environmental pollution damages to caused by skin, it is necessary to for the different skin damage mechanisms of pollution sources, is added in skin care item more Kind functional component.But the active component with antipollution effect, it is mostly unstable, it is more particular against the composition of oxidative damage With reproducibility, during storage and use easily and air contact, it is oxidized by oxygen and loses activity, or even color change occur Deep situation.Also also there is the defects of color is deep, smell is heavier in some active components, if these active components are directly added into Into skin care item, can cause skin care item lotion color unsightly, fragrance the problems such as being difficult to receive, influence use feeling.By above-mentioned Most of the limitation of factor, the existing skin care item with antipollution effect can only be from some side in cleaning, isolation, maintenance Face is set about, and can not be resisted environmental pollution comprehensively and be injured to caused by skin, it is difficult to multiple antipollution is realized in same product Effect.

The content of the invention

The technical problem to be solved in the present invention is to provide a kind of preparation method of the microcapsules with antipollution effect, tool Have the advantages that stability is good, conveniently add, skin resistance varying environment pollution infringement can be helped.

In order to solve the above technical problems, the present invention provides a kind of preparation method of the microcapsules with antipollution effect, its It is characterised by using following steps：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 2 ~ 6:3~8:3~5:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract And brown algae polyphenols, antipollution active compound is used as after mixing；25 ~ 55^oUnder C water bath conditions, by the antipollution activearm The Arabic gum aqueous solution obtained by compound and step A mix, obtains mixed solution, the dry weight of the Arabic gum in the mixed solution and The mass ratio of antipollution active compound is 1 ~ 2.4：1；Yeast extract is added into the mixed solution as emulsifying agent, ferment The addition of female extract is the 2 ~ 8% of the mixed solution quality, 10 ~ 30min of ultrasonic emulsification；Then under agitation, add Enter aqueous gelatin solution obtained by step A, the mass ratio of gelatin dry weight and Arabic gum dry weight is 1 ~ 3 after addition:1, finally add Mass concentration be 1% acetum regulation system pH to 3.8 ~ 4.3, under 600 ~ 1500rpm rotating speeds aggregation 30 ~ 90min；Continue stirring and be cooled to room temperature；The mass content of phenylpropyl alcohol alkanes material in the summer oak root extract is higher than 5%；Institute The 7- hydroxymatairesinols mass content stated in Norway spruce leaf extract is more than 2%；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 3 ~ 8% of step B resulting solution quality, then uses mass concentration For 10% NaOH solution regulation system pH to 8 ~ 9,30-60min is stirred at 1500 rpm, is then stopped stirring, is stood micro- Capsule sedimentation liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.

Gelatin of the present invention, INCI names：Gelatin, it is purchased from TRI-K Galaxy companies, trade name Colla-Gel AC；

Arabic gum of the present invention, INCI names：Arabic gum natural gum, is purchased from Sen Xin companies, trade name Natpure Gum.

The present invention is using yeast extract as emulsifying agent, INCI names：Yeast extract,《Cosmetic material name is used Claim catalogue（2015 editions）》Numbering：03469, it is purchased from OZEKI companies, trade name OZ-300U.

Summer oak root extract of the present invention, INCI names：Summer oak root extract,《Cosmetic material Names Catalogue is used （2015 editions）》Numbering：06947, reversibly prevent polycyclic aromatic hydrocarbon（PAHs）Representative substances --- benzo (a) pyrene and skin Aromatic hydrocarbon receptor in skin cell（AhR）With reference to avoiding the expression of CYP1A1 enzymes, and reactive oxygen species（ROS）With dihydroxy epoxy benzene And pyrene（BPDE）Generation.Because ROS can trigger skin inflammation, accelerate skin ageing, BPDE can cause nothing by being combined with DNA The DNA damage of method reparation, therefore using summer oak root extract as one of composition of antipollution composition, excellent isolation can be played And the effect of defence.

Summer oak root extract of the present invention is purchased from PRINCIPIUM companies of Switzerland, the phenylpropyl alcohol in the summer oak root extract The content of alkanes material is higher than 5%, and the percentage is mass percent.

Isobide dicaprylate of the present invention, CAS 64896-70-4, it is a kind of work that effect is repaired with barrier Property molecule, it can promote Caspase -14（Caspase-14）Expression.Caspase-14 with The formation of silk polyprotein is closely related, and the keratin fiber beam that intermediate filament polyprotein and keratin are cross-linked to form is skin barrier The pillar of " brick " structure；Silk polyprotein can also further be disintegrated generation NMF（NMF）, NMF can absorb moisture, so as to Horn cell gap is reduced, strengthens tight ness rating, prevents the intrusion of extraneous harmful substance or anaphylactogen.In addition, isobide two is pungent Acid esters can also promote the synthesis of tight junction protein, and tight junction protein can closely connect flanking cell, limit space between cells water Circulation, it is ensured that the sealing between organizing, realize the consolidation and recovery of epidermis barrier function.Isobide two of the present invention is pungent Acid esters is purchased from Sytheon companies, trade name：HydraSynol^TM DOI

Norway spruce leaf extract of the present invention, INCI names：Norway spruce leaf extract,《Cosmetic material title is used Catalogue（2015 editions）》Numbering 04915, there is excellent anti-oxidation efficacy, can effectively remove the free radical and active oxygen in skin Cluster, the skin inflammation and cellular damage for avoiding it from triggering.Moreover it is possible to suppress the activity of TYR enzyme, avoid ultraviolet and Pigmentation caused by environmental pollution.

7- hydroxymatairesinols content in Norway spruce leaf extract of the present invention is more than 2%, and the percentage is Mass percent.

Brown algae polyphenols are the secondary metabolites of brown alga, and its basic structural unit is phloroglucin, are a kind of natural antioxygens Agent and free radical scavenger.Brown algae polyphenols on the one hand can complexation of metal ions, on the other hand can also protect enzyme in human body, thin After birth, extracellular matrix etc. are from PM2.5 and O₃Infringement, Skin Cell is played integral protection effect.It is of the present invention The purity of brown algae polyphenols is more than 85%, and the percentage is mass percent.

The present invention uses gelatin, for wall material, using antipollution composition as core, to pass through complex coacervation legal system with Arabic gum For the microcapsules of chondritic are gone out, by the control to preparation technology, acquisition can wrap up summer oak root extract, different sorb simultaneously Alcohol dicaprylate, Norway spruce leaf extract, the microcapsules of four kinds of oil soluble active ingredients of brown algae polyphenols, prepare gained microcapsules Average grain diameter be 210.18 μm ~ 382.4 μm., can be after emulsification cools directly in the preparation process of antipollution skin care item Added in formula, preparation technology is simplified, while not oxidized protection functional component, reduction active matter color and gas can be played The advantages of influence of the taste to skin care item appearance property.

Failure mechanism of the present invention for all kinds of pollution factors to skin, by summer oak root extract, the octanoic acid of isobide two Ester, Norway spruce leaf extract, brown algae polyphenols are coated in microcapsules simultaneously according to special ratios, compared with prior art, tool Have the advantage that：1）Energy complexation heavy metal ion, and effectively avoid AhR from being combined generation toxic-complex PAH- with PAHs AhR, so as to hinder migration of the pollutant to nucleus, protect cells from damaging；2）Can by promoting the generation of GAP-associated protein GAP, Tough skin barrier, the ability of enhancing skin resistance environmental contaminants invasion and attack；3）Internal free radical and activity can be removed in time Oxygen cluster, inflammatory aging and pigmentation caused by reducing environmental pollution；4）Skin invading from ozone and ultraviolet can be protected Evil.Each composition Synergistic, there is comprehensive antipollution effect.

To prove the stability of microcapsules of the present invention, following contrast experiment is carried out：Mass concentration is 10% antipollution Active compound（Composition is the same as embodiment 2）Glycerite, to be light yellow, after placing 4 weeks under the conditions of the non-lucifuge of room temperature, color It is changed into dark-brown；And the antipollution active compound of phase homogenous quantities（Composition is the same as embodiment 2）, after encapsulation, identical Under condition of storage, color change is had no after 4 weeks.Microcapsules preserve three months under 40 DEG C of environment and are basically unchanged color, do not there is precipitation； Sample centrifuges 30min in 10000rpm centrifuge and has no precipitation；Show that wrapped antipollution active compound is not released Put, microcapsule stability is excellent.

To prove that antipollution active compound and microcapsules of the present invention have antipollution effect, tested as follows：

1st, damage of benzo (a) pyrene to DNA is reduced

Comet is a kind of quick, simple, directly detection DNA damage means.Using standardized human body's keratinocyte as experiment pair As being separately added into the antipollution active compound solution of mass fraction 1%, 3%, 5% in test group 1/2/3 and being cultivated, control group is used Isometric physiological saline processing, each group cell add 10% benzo (a) pyrene solution, comet are carried out after 24h.Wherein, anti-soil The proportioning of dye composition is shown in embodiment 2.

Cellular damage degree is classified in the amount of " tail of a comet cell " afterbody according to DNA.0 grade：<5%, not damaged, carefully Born of the same parents are without hangover；I levels：5% ~ 20%, low-grade trauma, there is a small amount of hangover；II levels：20% ~ 40%, moderate lesion, there is obvious hangover； III level：40% ~ 95%, high injury, there is serious hangover；IV levels：>95%, severe injury, turn into fragment.According to above-mentioned classification Index is observed and is classified to the degree of injury of each group cell, experimental result such as table 1.Illustrate antipollution activity of the present invention Composition can reduce damage of representative substances benzo (a) pyrene of polycyclic aromatic hydrocarbon to cell DNA, and then reduce because environmental pollution is led The skin of cause is damaged or aging.

The frequency disribution and percentage of the cometal cells of table 1 classification

2nd, skin barrier function is recovered

Environmental pollution can cause skin barrier function to be damaged, and its main performance characteristic is through transepidermal water loss value（TEWL values）Compared with It is high.Choose 30 to hang up one's hat in the more serious Pekinese subject of pollution condition, subject is without skins such as erythema, furfurs Rash, and without other dermatopathies or systemic disease, other skin-protection products are stopped using during test.30 subjects are divided into Two groups, every group of 15 people.After wherein the subject of test group cleans face skin by daily method daily, Yu Zao, evening smear addition Have 3%（Mass fraction）Having the face cream product of the microcapsules of antipollution effect described in embodiment 2, control group is then same using discrete phase, But the face cream of microcapsules is not added.Respectively at the 0th, 1,2,4 week measurement TEWL value and statistical analysis is carried out, to assess it to screen Hinder recovery effect of function, acquired results such as table 2.

After continuous use 4 weeks, the TEWL values that test group subject measures reduce by 22.5%, and have significant difference（p< 0.05）, and control group does not have significant difference before and after using（p>0.05）.Show have antipollution effect described in this patent Microcapsules can significantly repair the skin barrier caused by environmental pollution and be damaged, tough skin barrier, and enhancing skin resistance environment is dirty The ability of dye.

Table 2 is using test zone before and after antipollution skin care item through transepidermal water wastage

In summary, core, wall material and the emulsifying agent of present invention selection special ratios, by special process, acquisition can wrap simultaneously Wrap up in summer oak root extract, isobide dicaprylate, these four antipollution activity of Norway spruce leaf extract and brown algae polyphenols into The stable microcapsules divided.On the one hand, the physical isolation layer of microcapsules can effectively avoid the Oxidative demage of air, and active component is risen To good protective effect；On the other hand, the active component after parcel, the color and smell of itself are to cosmetic base lotion Obvious influence is not had.The microcapsules for being enclosed with a variety of antipollution active components are added directly into the lotion of skin care item basis, In use, microcapsules finger be coated with lotion when pressure under rupture, active ingredient release, can guarantee that product using when still have Higher activity concentration, so as to preferably play its skin-care effect.

Embodiment

With reference to specific embodiment, the present invention will be further described, but the invention is not limited in following examples.

Embodiment 1：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 2:5:3:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract and brown alga Polyphenol, antipollution active compound is used as after mixing；25^oUnder C water bath conditions, by the antipollution active compound and step Arabic gum aqueous solution mixing obtained by A, obtains mixed solution, the dry weight and antipollution active component of the Arabic gum in mixed solution The mass ratio of thing is 1:1；Yeast extract is added into the mixed solution is as emulsifying agent, the addition of yeast extract The 8% of the mixed solution quality, ultrasonic emulsification 15min；Then under agitation, aqueous gelatin solution obtained by step A is added, The mass ratio of gelatin dry weight and Arabic gum dry weight is 1 after addition:1, finally add the acetum that mass concentration is 1% and adjust Section system pH to 3.8, the aggregation 90min under 600rpm rotating speeds；Continue stirring and be cooled to room temperature；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 6% of step B resulting solution quality, is then with mass concentration 10% NaOH solution regulation system pH to 8 ~ 9, stirs 30min at 1500 rpm, then stop stirring, stand microcapsules sink Descending liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.

Embodiment 2：

A kind of preparation method of the microcapsules with antipollution effect：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 4:6:4:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract and brown alga Polyphenol, antipollution active compound is used as after mixing；45^oUnder C water bath conditions, by the antipollution active compound and step Arabic gum aqueous solution mixing obtained by A, obtains mixed solution, the dry weight and antipollution active component of the Arabic gum in mixed solution The mass ratio of thing is 1.4:1；Yeast extract is added into the mixed solution as emulsifying agent, the addition of yeast extract For the 6.3% of the mixed solution quality, ultrasonic emulsification 20min；Then under agitation, it is water-soluble to add gelatin obtained by step A Liquid, the mass ratio of gelatin dry weight and Arabic gum dry weight is 1.6 after addition:1, it is molten finally to add the acetic acid that mass concentration is 1% Liquid regulation system pH to 4.0, the aggregation 70min under 800rpm rotating speeds；Continue stirring and be cooled to room temperature；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 8% of step B resulting solution quality, is then with mass concentration 10% NaOH solution regulation system pH to 8 ~ 9, stirs 45min at 1500 rpm, then stop stirring, stand microcapsules sink Descending liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.

Embodiment 3：

A kind of preparation method of the microcapsules with antipollution effect：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 6:8:5:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract and brown alga Polyphenol, antipollution active compound is used as after mixing；35^oUnder C water bath conditions, by the antipollution active compound and step Arabic gum aqueous solution mixing obtained by A, obtains mixed solution, the dry weight and antipollution active component of the Arabic gum in mixed solution The mass ratio of thing is 1.8:1；Yeast extract is added into the mixed solution as emulsifying agent, the addition of yeast extract For the 4.6% of the mixed solution quality, ultrasonic emulsification 10min；Then under agitation, it is water-soluble to add gelatin obtained by step A Liquid, the mass ratio of gelatin dry weight and Arabic gum dry weight is 2.3 after addition:1, it is molten finally to add the acetic acid that mass concentration is 1% Liquid regulation system pH to 3.9, the aggregation 50min under 1000rpm rotating speeds；Continue stirring and be cooled to room temperature；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 3% of step B resulting solution quality, is then with mass concentration 10% NaOH solution regulation system pH to 8 ~ 9, stirs 60min at 1500 rpm, then stop stirring, stand microcapsules sink Descending liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.

Embodiment 4：

A kind of preparation method of the microcapsules with antipollution effect：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 3:3:5:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract and brown alga Polyphenol, antipollution active compound is used as after mixing；50^oUnder C water bath conditions, by the antipollution active compound and step Arabic gum aqueous solution mixing obtained by A, obtains mixed solution, the dry weight and antipollution active component of the Arabic gum in mixed solution The mass ratio of thing is 2.2:1；Yeast extract is added into the mixed solution as emulsifying agent, the addition of yeast extract For the 2.8% of the mixed solution quality, ultrasonic emulsification 25min；Then under agitation, it is water-soluble to add gelatin obtained by step A Liquid, the mass ratio of gelatin dry weight and Arabic gum dry weight is 2.6 after addition:1, it is molten finally to add the acetic acid that mass concentration is 1% Liquid regulation system pH to 4.2, the aggregation 40min under 1250rpm rotating speeds；Continue stirring and be cooled to room temperature；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 5% of step B resulting solution quality, is then with mass concentration 10% NaOH solution regulation system pH to 8 ~ 9, stirs 50min at 1500 rpm, then stop stirring, stand microcapsules sink Descending liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.

Embodiment 5：

A kind of preparation method of the microcapsules with antipollution effect：

A. the preparation of glue：Certain mass gelatin is weighed, is dissolved in distilled water, is heated to 50^oC, use IKA agitators 1500rpm is stirred, and until dissolving, is configured to the aqueous gelatin solution that mass fraction is 5%；Weigh certain mass Arabic gum in 80^oIn C distilled water, stirred using IKA agitators 1500rpm, until dissolving, be configured to the Arabic glue that mass fraction is 5% Solution；Two kinds of glues are 40^oC insulations are standby.

B. the preparation of microcapsules：By 5:4:3:1 mass ratio weighs summer oak root extract, isobide dicaprylate, moved Prestige dragon spruce leaf extract and brown algae polyphenols, form antipollution active compound；55^oUnder C water bath conditions, step A is prepared The 5% Arabic gum aqueous solution is mixed to form mixed liquor with antipollution active compound, and the wherein dry weight of Arabic gum is lived with antipollution Property composition mass ratio be 2.4:1；Then the yeast extract for accounting for mixed liquor mass ratio 2% is added as emulsifying agent, ultrasound breast Change 30min；Add 5% aqueous gelatin solution that step A is prepared after emulsification into mixed liquor while stirring, addition should meet gelatin Dry weight ratio with Arabic gum in mixed liquor is 3:1；With 1% acetum regulation system pH to 4.3 after charging, Aggregation 30min under 1500rpm rotating speeds.

C. the solidification of microcapsules：Treat that the solution that step B obtains naturally cools to room temperature, maintain IKA agitators 1500rpm Stirring, is placed in cold bath, maintains solution temperature 5 ~ 10^oBetween C, add and analyze pure formalin（Formaldehyde quality point Number is 37%）Crosslinking curing is carried out, addition is the 4% of step B resulting solution（Count in mass ratio）, and adjusted with 10%NaOH solution Section system pH to 8 ~ 9, keep stirring 40min under IKA agitators 1500rpm, it is rear to stop stirring, stand complete to the microcapsules formed Bulk deposition.

D. the filtering and cleaning of microcapsules：The above-mentioned mixed liquor containing microcapsules is positioned over 295-108 type polyvinyl filter clothes On filtered, the microcapsules containing antipollution active component are produced on filter cloth.Microcapsules are washed repeatedly with deionized water, and are adopted With content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until content of formaldehyde less than 100 ppm is clear in eluate Wash terminal.Finally microcapsules are placed in German WT BINDER vacuum drying chambers, in 25 ~ 35^oC, relative vacuum pressures- Dried 24 hours under 0.08Mpa, that is, obtain the microcapsules with antipollution effect.

Claims (1)

1. a kind of preparation method of the microcapsules with antipollution effect, it is characterised in that using following steps：

A, in mass ratio 1:20 weigh gelatin, distilled water, and gelatin is added in distilled water, is heated to 50^oStirred under C, 1500rpm Mix to dissolving, obtain aqueous gelatin solution；In mass ratio 1:20 weigh Arabic gum, distilled water, and Arabic gum is added into distilled water In, it is heated to 80^oStirring obtains the Arabic gum aqueous solution to dissolving under C, 1500rpm；Institute's gelatin water solution, Arabic glue Solution is 40^oIt is incubated under C standby；

B, in mass ratio 2 ~ 6:3~8:3~5:1 weighs summer oak root extract, isobide dicaprylate, Norway spruce leaf extract And brown algae polyphenols, antipollution active compound is used as after mixing；25 ~ 55^oUnder C water bath conditions, by the antipollution activearm The Arabic gum aqueous solution obtained by compound and step A mix, obtains mixed solution, the dry weight of the Arabic gum in the mixed solution and The mass ratio of antipollution active compound is 1 ~ 2.4：1；Yeast extract is added into the mixed solution as emulsifying agent, ferment The addition of female extract is the 2 ~ 8% of the mixed solution quality, 10 ~ 30min of ultrasonic emulsification；Then under agitation, add Enter aqueous gelatin solution obtained by step A, the mass ratio of gelatin dry weight and Arabic gum dry weight is 1 ~ 3 after addition:1, finally add Mass concentration be 1% acetum regulation system pH to 3.8 ~ 4.3, under 600 ~ 1500rpm rotating speeds aggregation 30 ~ 90min；Continue stirring and be cooled to room temperature；The mass content of phenylpropyl alcohol alkanes material in the summer oak root extract is higher than 5%；Institute The 7- hydroxymatairesinols mass content stated in Norway spruce leaf extract is more than 2%；

C, the solution obtained by step B is placed in 5 ~ 10 under 1500rpm stirrings^oIn C cold baths, it is 37% to add mass concentration Formalin carries out crosslinking curing, and the addition of formalin is the 3 ~ 8% of step B resulting solution quality, then uses mass concentration For 10% NaOH solution regulation system pH to 8 ~ 9,30-60min is stirred at 1500 rpm, is then stopped stirring, is stood micro- Capsule sedimentation liquid；

D., microcapsules sedimentation liquid obtained by step C is positioned on 295-108 type polyvinyl filter clothes and filtered, by the filter on filter cloth Go out thing to be washed repeatedly with deionized water, and with content of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry eluate, until eluate Middle content of formaldehyde is less than 100 ppm, stops cleaning, the much filtrate is placed in vacuum drying chamber, 25 ~ 35^oC, relatively very Dried 24 hours under pneumatics power -0.08Mpa, produce the microcapsules with antipollution effect.