CN105982823A - Aqueous-dispersible boron nitride powder for cosmetics and preparation method thereof - Google Patents
Aqueous-dispersible boron nitride powder for cosmetics and preparation method thereof Download PDFInfo
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- CN105982823A CN105982823A CN201610249204.8A CN201610249204A CN105982823A CN 105982823 A CN105982823 A CN 105982823A CN 201610249204 A CN201610249204 A CN 201610249204A CN 105982823 A CN105982823 A CN 105982823A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
Abstract
The invention discloses aqueous-dispersible boron nitride powder for cosmetics and a preparation method thereof. The method comprises the following steps: pre-dispersing synthesized hexagonal boron nitride coarse powder which serves as a raw material in a surfactant aqueous solution, and performing surface activation by means of equipment grinding; centrifuging, washing, and adding the supernatant powder on a filter screen into the hydrophilic surfactant solution for surface modification, drying, grinding and screening to obtain the aqueous-dispersible boron nitride powder. The powder has excellent dispersibility in water, is applicable to oil-in-water cream/emulsion, skin-protecting gel, facial mask essence, lotion(spray), sunscreen spray, hair-care products and other non-rinse-off products, has the effects of improving skin smoothness, promoting fine, white and other makeup, and is an excellent cosmetic additive raw material.
Description
Technical field
The present invention relates to a kind of water-dispersible boron nitride powder used for cosmetic and preparation method thereof, belong to surface modification cosmetics
Material Field, it is intended to improve the application in water base cosmetics series of the hydrophobic hexagonal boron nitride and stability thereof, finally make
The standby water-dispersible boron nitride powder obtained all meets the requirement of China's " cosmetics health specification " 2007 editions, this preparation method technique
Simple easily production.
Background technology
About in 1940, hexagonal boron nitride is applied in cosmetics by Japan first, but a very long time is all worked as
Becoming luxury goods, along with the development of synthetic technology is with universal, the synthesis of hexagonal boron nitride is not the most the thing of part difficulty, cost
Reducing makes boron nitride must give substantial amounts of application in cosmetics.In the product of almost all of leader's cosmetic industry, such as: powder
In cake, loose powder, foundation cream, eye-liner, eye shadow, rouge, lipstick and substantial amounts of skin care item, all using boron nitride.The graphite of stratiform
Type crystal structure, Mohs' hardness 2Gpa and low to 0.16 coefficient of friction, higher oil absorption and water tariff collection and prevent skin from doing
Split ability, lubricity, excellent ductility, the sense of touch of pleasant and performance of persistently fixing, the refraction index as silk is soft
1.74 close to human body skin, soft light scattering, vertical aobvious " naked shape effect " after having made adornment.It is Traditional makeup powder body raw material,
As: materials such as Pulvis Talci, titanium dioxide, mica powder, nylon powder, silica flour, glass dust, polyethylene powder incomparable.
As the synthetically produced method of hexagonal boron nitride powder, a lot of patent documentation of a lot of units is all described, various sides
Formula can produce excellent hexagonal boron nitride powder.
Along with the expansion of hexagonal boron nitride range of application, the use limitation of boron nitride the most increasingly comes out.Six sides
Boron nitride surface does not contains hydrophilic group, shows stronger hydrophobic performance, and light weight is easier to swim on the water surface, adds lamellar structure
Easily the water surface sprawls film forming, adds hexagonal boron nitride dispersion difficulty in water.Make hexagonal boron nitride at water base cosmetics body
Application in system is limited.Even if high force dispersion adds in emulsifying cream formula, powder body easily assemble in aqueous based systems agglomerating and
Flocculate coarse.Stability under long-time formula is investigated is the poorest so that technological development personnel to hexagonal boron nitride at aqueous based systems
In application bring difficulty.Now the research in the water-dispersible performance of hexagonal boron nitride is the most rare, particularly can meeting
The water-dispersible boron nitride of cosmetic.
At present boron nitride powder Research on Surface Modification, such as: application publication number CN102786815A boron nitride surface modification and
Polymer composites, in terms of hexagonal boron nitride modification, grafting cosmetics disagreeableness polymeric materials, to skin, skin
Sense produces injury, forbids adding in cosmetic formulations.The activation on application publication number CN101715611A boron nitride surface, allows
Boron nitride has carried out surface active, it is therefore an objective to improve proton-conducting, uses answering of fuel cell, electrolysis bath or accumulator
With.Application publication number CN104684844A hydrophilic/high oil-absorbing boron nitride powder and manufacture method thereof and cosmetic preparation, be to allow
The modification of boron nitride strengthens the persistency of dressing in cosmetic process, not the application in aqueous based systems.Most of boron nitride
Research and development the most fundamentally solve the water-dispersible performance of boron nitride in cosmetics and at aqueous based systems cosmetics
The stability of middle application.
Summary of the invention
For above-mentioned existing hexagonal boron nitride cosmetics aqueous based systems application present in problem, the main mesh of the present invention
Be to provide the preparation method of a kind of hexagonal boron nitride surface hydrophilic modification, this method low cost, operating procedure are simple, condition
Controllability is strong；While hexagonal boron nitride hydrophilic and water dispersible are resolved, improve stablizing of products application further
Performance so that with the addition of the cosmetics such as cream, emulsion that water-dispersible hexagonal boron nitride manufactures, homogeneous, the most coarse, no
Floc sedimentation.
In order to achieve the above object, the present invention adopts the following technical scheme that, the step of preparation method is as follows:
(1) with synthesis hexagonal boron nitride coarse powder as raw material, be pre-dispersed in the aqueous solution of surfactant；
(2) grind by equipment and the raw material in surfactant aqueous solution is ground and soaks surface activation process；
(3) raw material after activation is centrifuged, repeatedly rinses and filter；
(4) take drainage screen upper strata powder to join in the hydrophilic surface modification agent solution of stirring and carry out hydrophilic modifying；
(5) modified powder is dried, pulverizes, sieved, prepare water-dispersible hexagonal boron nitride powder.
In step (1), selected hexagonal boron nitride raw material is coarse powder particles, and then strong stirring is dispersed in PH≤3
Surfactant aqueous solution in activate.Hexagonal boron nitride coarse powder, maintains hexagonal boron nitride more in building-up process
In the original interface of disposable crystal grain, be ground pulverizing in the presence of surfactant, newly generated to powder body
The interface gone out carries out being coated with and disperseing, promote later stage activation effect, puts into than the powder body being crushed to target grain size in advance again
Effect in surface active solution to be got well.Surfactant used is: the one in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid or its group
Close.
In step (2), it is broken into mean diameter by grounds travel and reaches 2-30 micron particulate powders, this particle diameter six side's nitrogen
The interface of change boron is increased, the breaking bonds of boron nitride also increases.The ground hexagonal boron nitride slurry containing activator is placed on storage tank
Middle continuation activates 12-48 hour, and the time, too short then activation effect was bad, and overlong time then affects production efficiency.Milling apparatus is:
The medium one of ball mill, colloid mill, high speed dispersor or combination.
In step (3), the hexagonal boron nitride slurry suction centrifuge of activator will be contained after grinding, use deionized water
Repeatedly rinse to lower floor's filtrate pH value in the range of 5-7, it is therefore an objective to make the outer activator solution brought into and dirt solution the most clear
Washing complete, on the other hand, rational pH range and low impurity content are also more suitable in cosmetics adding use, unlikely
Stimulate in skin is produced.
In step (4), take the upper strata powder activated, join in the pre-dispersed solution of surface modifier, dispersed with stirring
Become pasty state, hydrophilic surface modification agent: powder body: water=0.3-1:10-20:20-30.Described hydrophilic surface modification agent is: PEG-8
Polydimethylsiloxane, PEG-12 polydimethylsiloxane, ammonia end polydimethylsiloxane, the one of PEG-4000 or group
Close.Selected hydrophilic surface modification agent and powder body and the ratio of water are the dispersibility according to the water-dispersible boron nitride powder later stage and answer
The consumption determined by stability, inorganic agent crosses and do not reaches good dispersion and stablizing effect at least, and inorganic agent is too much, then powder body
Sticky the most agglomerating, in cosmetic formulations, use can too much produce the physicochemical characteristic of inorganic agent, brings impact to use.
In step (5), modified good powder is put into a thin layer that tiles respectively in frame and puts into oven for drying, then pulverize,
Sieve, the water-dispersible boron nitride powder finally given, meet 2007 editions required every fingers of China's " cosmetics health specification "
Mark.The method pulverized simply is broken up the aggregate drying caking and is pulverized without high intensity, does not produce new interface；Sieve and adopted
Screen cloth model be 200 mesh, residue on sieve continues to pulverize and sieve.
The water-dispersible hexagonal boron nitride powder that the present invention obtains, in water, wetting and dispersing can be excellent, for cosmetics water bag
The non-rinse-off products such as ointment frost/emulsion, skin-care gel, mask elite, surfactant (spraying), sunscreen spray, hair product
In, there is easily interpolation, easily disperse, the product worked it out is stable, and mastic is homogeneous does not return thick advantage.
The used for cosmetic water-dispersible boron nitride powder that will obtain based on above-mentioned preparation method, has expanded hexagonal boron nitride and has existed
The range of application of cosmetics aqueous based systems.
Accompanying drawing explanation
Table 1 each Example formulations composition and evaluation.
Fig. 1 is process chart prepared by the used for cosmetic water-dispersible boron nitride powder that the present invention designs.
Fig. 2 is to illustrate the water-dispersible hexagonal boron nitride powder water in common hexagonal boron nitride powder (left) and embodiment 1
Dispersion comparison figure (right).
Fig. 3 is to illustrate the water-dispersible hexagonal boron nitride powder water in common hexagonal boron nitride powder (left) and embodiment 2
Angle of wetting comparison figure (right).
Fig. 4 is that the water-dispersible hexagonal boron nitride powder in embodiment 3 is distributed feelings in formula coding ZSQ15092103 cream
The electron micrograph figure of condition.
Fig. 5 is that the water-dispersible hexagonal boron nitride powder in embodiment 4 is distributed feelings in formula coding ZSQ15092104 cream
The electron micrograph figure of condition.
Fig. 6 is that the water-dispersible hexagonal boron nitride powder in embodiment 5 is distributed feelings in formula coding ZSQ15092105 cream
The electron micrograph figure of condition.
Fig. 7 is that the water-dispersible hexagonal boron nitride powder in embodiment 6 is distributed feelings in formula coding ZSQ15092106 cream
The electron micrograph figure of condition.
Fig. 8 is that the water-dispersible hexagonal boron nitride powder in embodiment 7 is distributed feelings in formula coding ZSQ15092107 cream
The photo figure of the general camera of condition.
Fig. 9 is common hexagonal boron nitride powder electronic display of distribution situation in formula coding ZSQ15092108 cream
Micro mirror photo figure.
Detailed description of the invention
In order to the present invention is expanded on further, illustrate in conjunction with following implementation:
1. preparation process is as follows:
(1), under room temperature, 10 grams of boron nitride coarse powder are weighed.
(2) weigh commercially available surfactant and make an addition in 100 grams of deionized waters, the dilute acid soln of preparation PH≤3.0.
(3), under quickly stirring, the boron nitride powder in above-mentioned steps (1) is dispersed in the weak solution of step (2), obtains
Boron nitride pre-dispersed liquid.
(4) dispersion liquid of step (3) boron nitride powder is first passed through colloid mill and pumps into the sand mill of high-speed circulating operating again
In, being ground to mean diameter is 2-30 micron.
(5) by bn slurry good for step (4) sand milling, within standing 48 hours under room temperature.
(6) slurry after step (5) being activated is centrifugal in centrifuge, repeatedly rinses with deionized water, exists to filtrate PH
5.0-7.0 left and right.
(7), under room temperature, weigh 0-0.6 gram of hydrophilic modifying agent and be dispersed in 20 grams of deionized waters, pre-dispersed uniformly, by step
(6) in, centrifugal upper strata powder stirs into homogeneous paste with hydrophilic modifying pre-dispersed liquid.
(8) by the pastel in step (7), paving frames up puts into drying in baking oven..
(9) powder after step (8) being dried is pulverized, then sieves with 200 mesh, obtains final products.
2. according to the specific operation process of above water-dispersible boron nitride used for cosmetic, point 6 embodiments introduce the present invention, real
Execute each variable parameter of example as follows:
Table 1 each Example formulations composition and evaluation
Continuous upper table
The most each embodiment preparation technology:
After being weighed by A phase constituent, it is heated to 80 ~ 85 DEG C, dissolves completely.
Being added to the water after B phase being weighed, be wherein added to the water after HANSHENGJIAO and glycerol premixing, stirring mixing heats up
To 80 ~ 85 DEG C.
A is added in B phase under stirring, quickly stirring homogenizing 3 ~ 5 minutes, water-bath insulation froth breaking about 5 minutes.
Stirring cooling after froth breaking.
When being cooled to about 70 DEG C, add C phase and neutralize；Cool to 55-65 DEG C, add pre-dispersed good D phase.
Being cooled to when 50 DEG C add E phase, stirring is cooled to discharging when 35-40 DEG C.
Seeing Fig. 2, it show the one water-dispersible nitridation used for cosmetic that this example 1 shot by camera is prepared
Boron powder body in water naturally dispersion situation (right) with not through surface hydrophilic modification process hexagonal boron nitride in water oneself
So disperse the contrast photo of situation (left), it is found that not through the boron nitride of hydrophilic surface modification, show strong hydrophobic
Performance, floats on the water surface, nonwetting.And through the water-dispersible boron nitride of this instance processes, in water, wetting effect is good, suspend
Stable dispersion is uniform.
Seeing Fig. 3, it show the water-dispersible boron nitride powder dropping water that this example 2 shot by camera is prepared
Angle of wetting situation (right) with through surface hydrophilic modification process hexagonal boron nitride dropping water angle of wetting situation (left)
Contrast photo, it is found that not through the boron nitride of hydrophilic surface modification, globule glomeration, powder drying does not absorbs water.And
Through the water-dispersible boron nitride of this instance processes, water one instills, and is just given by boron nitride powder and absorbs, the globule easily moistening powder body.
Seeing Fig. 4, it show the water-dispersible boron nitride powder that this example 3 shot by optical microscope is prepared
Body, at following effect example: distribution situation microphotograph in laboratory coding zsq15092103 cream, this embodiment 3 is made
Standby water-dispersible boron nitride powder dispersibility in mastic out is good, and mastic texture is uniform, and centrifugal nothing of investigating sinks to the bottom, makeup
Smear use light fine and smooth.
Seeing Fig. 5, it show the water-dispersible boron nitride powder that this example 4 shot by optical microscope is prepared
Body, at following effect example: the optical microscope photograph of distribution in laboratory coding zsq15092104 cream, this is real
Executing water-dispersible boron nitride powder dispersibility in mastic that example 4 prepares preferable, mastic texture is uniform, centrifugal investigates nothing
Sinking to the bottom, during upper shape smears use, light is fine and smooth.
Seeing Fig. 6, it show the water-dispersible boron nitride powder that this example 5 shot by optical microscope is prepared
Body, at following effect example: dispersibility microphotograph in laboratory coding zsq15092105 cream, prepared by this embodiment 5
Water-dispersible boron nitride powder good dispersion in mastic out, mastic texture ratio is more uniform, and centrifugal nothing of investigating sinks to the bottom, on
It is fine and smooth that shape smears use light.
Seeing Fig. 7, it show the water-dispersible boron nitride powder that this example 6 shot by optical microscope is prepared
Body, at following effect example: dispersibility microphotograph in laboratory coding zsq15092106 cream, prepared by this embodiment 6
The dispersibility in mastic of water-dispersible boron nitride powder out is preferable, and mastic texture ratio is more uniform, and centrifugal nothing of investigating sinks to the bottom,
It is fine and smooth that upper shape smears use light.
Seeing Fig. 8, it show the water-dispersible boron nitride powder that this example 7 shot by general camera is prepared,
At following effect example: the photo of distribution situation in laboratory coding zsq15092107 cream, this embodiment 7 prepares
Water-dispersible boron nitride powder dispersibility deviation in mastic, mastic outward appearance has slight granular sensation, centrifugal investigation slightly to sink to the bottom.
Participating in Fig. 9, it show the formula composition 8 shot by optical microscope, laboratory coding zsq15092108 cream
Without the microphotograph of hexagonal boron nitride distribution situation of hydrophilic surface modification in frost, boron nitride powder disperses in mastic
Sexual deviation, mastic texture is the most coarse, and centrifugal investigation sinks to the bottom, and upper shape smears use slight powder sense.
It is good that above example demonstrates the present invention water-dispersible boron nitride dispersibility in water, uses interpolation side in cosmetics
Just, improving stability and the using effect of formula, solve boron nitride difficult dispersion in water, the cosmetics at aqueous based systems are joined
Side is difficult to apply and is difficult to a stable difficult problem, be that a kind of excellent cosmetics add raw material.
Claims (9)
1. the preparation method of a water-dispersible boron nitride powder used for cosmetic, it is characterised in that described preparation method step is as follows:
(1) with synthesis hexagonal boron nitride coarse powder as raw material, be pre-dispersed in the aqueous solution of surfactant；
(2) grind by equipment and the raw material in surfactant aqueous solution be ground and soak surface activation process,
(3) raw material after activation is centrifuged, repeatedly rinses and filter；
(4) take drainage screen upper strata powder to join in the hydrophilic surface modification agent solution of stirring and carry out hydrophilic modifying；
(5) modified powder is dried, pulverizes, sieved, prepare water-dispersible hexagonal boron nitride powder.
Surfactant the most according to claim 1 is: hydrochloric acid, sulphuric acid, nitric acid, the one of phosphoric acid or combination.
Pre-dispersed pH value≤3 of hexagonal boron nitride surfactant aqueous solution the most according to claim 1.
Milling apparatus the most according to claim 1 is ball mill, colloid mill, the one of high speed dispersor or combination.
The hexagonal boron nitride powder mean diameter carrying out surface active after grinding the most according to claim 1 is: 2-30
Micron.
Immersion treatment in surfactant solution the most according to claim 1, soak time is: 12 to 48 hours.
Centrifugal, flushing the most according to claim 1, the PH of final lower floor filtrate controls in the range of 5-7.
Surface modifier the most according to claim 1 is: PEG-8 polydimethylsiloxane, PEG-12 polydimethylsiloxanes
Alkane, ammonia end polydimethylsiloxane, the one of PEG-4000 or combination.
9. a water-dispersible boron nitride powder used for cosmetic, it is characterised in that described water-dispersible boron nitride powder is wanted according to right
The preparation method according to any one of 1-9 is asked to prepare.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163290A (en) * | 2017-05-18 | 2017-09-15 | 清华-伯克利深圳学院筹备办公室 | A kind of functionalization boron nitride nanosheet and its preparation method and application |
| CN114132903A (en) * | 2021-01-08 | 2022-03-04 | 上海联锴日用化工有限公司 | Preparation method of hydrophilic nano boron nitride |
| CN115887248A (en) * | 2022-12-26 | 2023-04-04 | 广州联锴粉体科技有限公司 | Sunscreen product containing modified hexagonal boron nitride and preparation method thereof |
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| CN101715611A (en) * | 2007-05-28 | 2010-05-26 | 塞拉姆氢技术公司 | Method of activating boron nitride |
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN102985055A (en) * | 2010-05-07 | 2013-03-20 | 香奈儿香水美妆品公司 | Cosmetic composition comprising boron nitride complex powder |
| CN104684844A (en) * | 2012-09-28 | 2015-06-03 | 水岛合金铁株式会社 | Hydrophilic and highly oil-absorbent boron nitride powder, production method therefor, and cosmetic |
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2016
- 2016-04-20 CN CN201610249204.8A patent/CN105982823A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101715611A (en) * | 2007-05-28 | 2010-05-26 | 塞拉姆氢技术公司 | Method of activating boron nitride |
| CN102985055A (en) * | 2010-05-07 | 2013-03-20 | 香奈儿香水美妆品公司 | Cosmetic composition comprising boron nitride complex powder |
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN104684844A (en) * | 2012-09-28 | 2015-06-03 | 水岛合金铁株式会社 | Hydrophilic and highly oil-absorbent boron nitride powder, production method therefor, and cosmetic |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163290A (en) * | 2017-05-18 | 2017-09-15 | 清华-伯克利深圳学院筹备办公室 | A kind of functionalization boron nitride nanosheet and its preparation method and application |
| CN107163290B (en) * | 2017-05-18 | 2019-08-23 | 清华-伯克利深圳学院筹备办公室 | A kind of functionalization hexagonal boron nitride nanosheet, dispersion liquid and its preparation method and application |
| CN114132903A (en) * | 2021-01-08 | 2022-03-04 | 上海联锴日用化工有限公司 | Preparation method of hydrophilic nano boron nitride |
| CN115887248A (en) * | 2022-12-26 | 2023-04-04 | 广州联锴粉体科技有限公司 | Sunscreen product containing modified hexagonal boron nitride and preparation method thereof |
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Application publication date: 20161005 |