CN108360285A - The preparation method for adulterating the silk paper of Cellulose nanocrystal palpus and its application in facial mask - Google Patents
The preparation method for adulterating the silk paper of Cellulose nanocrystal palpus and its application in facial mask Download PDFInfo
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- CN108360285A CN108360285A CN201810051513.3A CN201810051513A CN108360285A CN 108360285 A CN108360285 A CN 108360285A CN 201810051513 A CN201810051513 A CN 201810051513A CN 108360285 A CN108360285 A CN 108360285A
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- silk
- cellulose nanocrystal
- fibroin
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/28—Organic non-cellulose fibres from natural polymers
- D21H13/34—Protein fibres
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/733—Alginic acid; Salts thereof
-
- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
- A61K8/988—Honey; Royal jelly, Propolis
-
- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/99—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from microorganisms other than algae or fungi, e.g. protozoa or bacteria
-
- 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
-
- 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
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
-
- 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
- A61Q19/08—Anti-ageing preparations
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/02—Synthetic cellulose fibres
Abstract
The invention discloses a kind of preparation method of silk paper of doping Cellulose nanocrystal palpus and its applications in facial mask.The preparation method of the silk paper includes the following steps：(1) centrifugation removes moisture after silk being carried out hot-water pretreatment, then carries out alkali process, then clean to neutrality, obtains fibroin fiber；(2) protease is added in the fibroin fiber obtained in step (1), is digested after being uniformly mixed, then the fibroin slurries obtained after enzymolysis are subjected to inactivation treatment, the fibroin slurries after being inactivated；(3) Cellulose nanocrystal must be added in the fibroin slurries after the inactivation obtained in step (2) and carries out copy paper, obtain the silk paper of doping Cellulose nanocrystal palpus.The silk paper of acquisition is impregnated into Essence in the present invention and obtains silk mask, which not only has good gas permeability and flexibility, but also has excellent water-retaining property and adsorptivity, and deep water supplement, the anti-wrinkle whitening of skin may be implemented.
Description
Technical field
The invention belongs to cosmetic field, more particularly to a kind of preparation method of the silk paper of doping Cellulose nanocrystal palpus
And its application in facial mask.
Background technology
With the progress of the development and science and technology of society, the raising of people’s lives level, pressure is also following, with pressure
Power and come be exactly skin it is in eclipse, do not have good soft and smooth careful, therefore more and more women is to face beautifying health keeping product
Increasingly favor.Facial mask has become a portion mostly important in skin care because nutritional ingredient height, skin care efficiency are notable
Point.The principle of facial mask is temporarily isolating extraneous air and pollution exactly using the of short duration time for being covered in face, improves skin
Temperature, the pore expansion of skin, promotes sweat gland secretion and metabolism, the oxygen content of skin is made to increase, and is conducive to skin exclusion
The oil substances of the product and accumulation of epidermal cell metabolism, the moisture in facial mask penetrate into the cuticula of epidermis, and skin becomes
Must be soft, skin is naturally bright flexible.Highest science and technology, carrier are careful at present, be easy to be inhaled by skin is silk mask.
As silk mask increasingly gets consumer reception, relevant patent is also more and more.Application No. is
The Chinese patent application of 201710092652.6, entitled " a kind of deep water supplement moisturizing silk mask and preparation method thereof " be with
Silk is base material, adds a variety of moisturizer, improves moisture preserving time, makes skin water profit penetrating, shines nature brilliance.Application No. is
201611050690.7, the Chinese patent application of entitled " a kind of anti-wrinkle anti aging effect silk mask and preparation method thereof " be
Using silk as base material, the old auxiliary agent of a variety of removing wrinkle and resisting agings is added, allows skin natural gloss, soft and smooth careful, delay skin aging.Application
Number for 201610297417.8, the Chinese patent application of entitled " a kind of maintenance type silk mask and preparation method thereof " be with silkworm
Silk is base material, containing abundant minerals and vitamin, improves cutaneous immunisation ability, while also having reparation effect to skin.Though
It says and states silk mask all with its unique effects, but absorption active ingredient ability is limited, most of Essence is not fine
Utilization, and silk mask generally use spinning moulding method be made, have certain limitation, therefore, it is necessary to research and develop tool
There is the composite facial mask of efficient whitening, anti-wrinkle and water supplement function to meet the demand in market.
Invention content
The primary purpose of the present invention is that the shortcomings that overcoming the prior art and deficiency, provide a kind of doping Cellulose nanocrystal
The preparation method of the silk paper of palpus.
Another object of the present invention is to provide the silk faces for the doping Cellulose nanocrystal palpus that the method is prepared
Paper.
It is still another object of the present invention to provide the applications of the silk paper of the doping Cellulose nanocrystal palpus.
The purpose of the invention is achieved by the following technical solution：A kind of preparation of the silk paper of doping Cellulose nanocrystal palpus
Method includes the following steps：
(1) centrifugation removes moisture after silk being carried out hot-water pretreatment, then carries out alkali process, then clean to neutrality, obtains
To fibroin fiber；
(2) protease is added in the fibroin fiber obtained in step (1), is digested after being uniformly mixed, then
The fibroin slurries obtained after enzymolysis are subjected to inactivation treatment, the fibroin slurries after being inactivated；
(3) Cellulose nanocrystal must be added in the fibroin slurries after the inactivation obtained in step (2) and carries out copy paper, obtained
To the silk paper of doping Cellulose nanocrystal palpus.
Hot water described in step (1) is preferably 95~100 DEG C of deionized water.
The condition of hot-water pretreatment described in step (1) is preferably：1~3h is handled in 95~100 DEG C of hot water.
The mass ratio of silk and water described in step (1) is preferably 1:(1~100).
The condition of centrifugation described in step (1) is preferably：3000rpm centrifuges 15min.
Alkali process described in step (1) is realized preferably by following steps：Silk is immersed in 80~100 DEG C, matter
Measure the Na that score is 0.1~10%2CO330~60min is reacted in solution, is then cleaned with 80~100 DEG C of water, again by it
Put into 80~100 DEG C, the Na that mass fraction is 0.1~10%2CO330~60min, repetitive operation 1~10 are reacted in solution
It is secondary；More preferably it is achieved by the steps of：By the Na that silk is immersed in 80~90 DEG C, mass fraction is 0.1~10%2CO3It is molten
30~60min is reacted in liquid, is then cleaned with 80~90 DEG C of water, is put into 80~90 DEG C, mass fraction 0.1 again
~10% Na2CO330~60min, repetitive operation 1~10 time are reacted in solution.
The mass ratio of the silk and sodium carbonate is preferably 100:(1~10).
Protease described in step (2) is Alealase 2.4L enzymes, papain, trypsase and Havorzyme
It is one or more of in protease；Preferably Alealase 2.4L enzymes.
The additive amount of protease described in step (2) is pressed to be calculated per g fibroin fiber proportioning 500~1500U protease.
The rotating speed of stirring described in step (2) is 100~1000r/min.
The condition of enzymolysis described in step (2) is preferably：4 are digested under conditions of pH is 6~9, temperature is 50~70 DEG C
~12h.
The condition of inactivation treatment described in step (2) is preferably：10~60min is kept the temperature in 80~100 DEG C of hot water；
The condition of inactivation treatment is more preferably：10~60min is kept the temperature in 80~90 DEG C of hot water.
The additive amount of Cellulose nanocrystal palpus described in step (3) must account for fibroin grind slurries quality by Cellulose nanocrystal
4%~20% calculates.
A kind of silk paper of doping Cellulose nanocrystal palpus, is prepared by method described in any one of the above embodiments.
Application of the silk paper of the doping Cellulose nanocrystal palpus in cosmetic field.
The cosmetics are preferably facial mask.
It is a kind of doping Cellulose nanocrystal must silk mask, by by above-mentioned doping Cellulose nanocrystal must silk paper
It is impregnated into Essence and obtains.
The Essence is preferably comprising aloe extract, purslane extract, yeast extract, glycine betaine, seaweed
The Essence of sour sodium and royal jelly extract.
The Essence further includes auxiliary agent.
The auxiliary agent includes moisturizer and antioxidant.
The moisturizer is in polyethylene glycol, glycerine, butanediol, Sodium Hyaluronate, triethanolamine and hydrolytic collagen
One or more.
The antioxidant is one kind in Phenoxyethanol and methyl hydroxybenzoate.
The Essence preferably comprises the following component counted in parts by weight：60 parts of water, 12 parts of glycerine, poly- second two
8 parts of alcohol, 0.2 part of Sodium Hyaluronate, 0.4 part of hydrolytic collagen, 8 parts of aloe extract, 3 parts of purslane extract, yeast extract 4
Part, 4 parts of glycine betaine, 2 parts of sodium alginate, 3 parts of royal jelly extract, 0.2 part of Phenoxyethanol.
The water is preferably deionized water.
The silk mask of the doping Cellulose nanocrystal palpus is applied in the fields such as cosmetics moisturizing, whitening, anti-wrinkle.
The present invention has the following advantages and effects with respect to the prior art：
1, the content of present invention obtains silk paper using wet papermaking technology, improves the manufacturing process of silk mask, reaches
Simplified technique, effect easy to operation.
2, the plant cellulose nano whisker that is added of the present invention has that specific surface area is high, modulus is big, and adsorption capacity is strong
Feature, make film have extremely strong gas permeability, good moisture holding capacity, it is extremely strong get close to skin, preferable adsorption capacity performance.
Facial mask is combined with Essence, can quickly adsorb the nutriment of Essence and is penetrated into skin, it is various to dispel
Cuticula repairs nourishes rough skin, allows skin freely to breathe, shines new vitality, and is free from side effects to skin and ill effect.
What 3, the present invention used is all the base material with biodegradability, will not be to environmental effects.Silkworm obtained
Silk facial mask not only has good gas permeability and flexibility, but also has excellent water-retaining property and adsorptivity, and skin may be implemented
Deep water supplement, anti-wrinkle whitening.
Description of the drawings
Fig. 1 is the preparation flow figure of the silk mask of present invention doping Cellulose nanocrystal palpus.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Alealase2.4L enzymes described in the embodiment of the present invention and comparative example are purchased from letter enzyme preparation company of Novi；Cellulose
Nano whisker is purchased from Shanghai Kai Xiang new materials Science and Technology Ltd., and aloe extract develops limited public affairs purchased from the intelligent section plant in Shaanxi
Department, purslane extract are purchased from Shaanxi Sen Fu natural products Co., Ltd, and royal jelly extract is purchased from the gloomy not natural product in Shaanxi
Co., Ltd, yeast extract are purchased from Xi'an Hao Yuan Bioisystech Co., Ltd, other raw materials and reagent can be from purchasing on the market
.
Essence involved in the present invention is grouped as by the group counted in parts by weight as follows：60 parts of deionized water, glycerine 12
Part, 8 parts of polyethylene glycol, 0.2 part of Sodium Hyaluronate, 0.4 part of hydrolytic collagen, 8 parts of aloe extract, 3 parts of purslane extract, ferment
4 parts of female extract, 4 parts of glycine betaine, 2 parts of sodium alginate, 3 parts of royal jelly extract, 0.2 part of Phenoxyethanol.
Embodiment 1
A kind of silk mask of doping Cellulose nanocrystal palpus, preparation method are as follows：
(1) silk raw material is added in 95 DEG C of water, is handled as 1h, the mass ratio of silk and deionized water is 1:1, centrifugation
Alkali process is carried out after dehydration.The centrifugation is carried out using flat centrifuge, and the condition of centrifugation is：Rotating speed is 3000rpm,
Centrifugation time is 15min.The alkali process is specially：By the Na that silk is immersed in 80 DEG C, mass fraction is 0.1%2CO3It is molten
It in liquid, after reacting 30min, is cleaned with 80 DEG C of deionized waters, puts into 80 DEG C again, the Na that mass fraction is 0.1%2CO3Solution
In, 30min is reacted, repeats 1 time, the fibroin fiber of acquisition is cleaned to neutrality；The wherein matter of silk and sodium carbonate
Amount is than being 100:1.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 800r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 50 DEG C, enzyme concentration is 500U/g substrates, pH is 6, digests 12h, take out 80
DEG C hot water in keep the temperature 10min, the fibroin slurries after being inactivated, by Cellulose nanocrystal must be added to inactivation after fibroin starch
Copy paper is carried out in liquid, obtains silk paper.Wherein Cellulose nanocrystal must account for the 4% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Embodiment 2
A kind of silk mask of containing cellulose nano whisker, preparation method are as follows：
(1) silk raw material is added in 95 DEG C of water, is handled as 3h, the mass ratio of silk and deionized water is 1:100, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 85 DEG C, mass fraction is 10%2CO3In solution, after reacting 60min, with 85 DEG C
Deionized water is cleaned, and puts into 85 DEG C again, the Na that mass fraction is 10%2CO3In solution, 60min is reacted, is repeated 5 times,
The fibroin fiber of acquisition is cleaned to neutrality.Wherein the mass ratio of silk and sodium carbonate is 100:10.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 200r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 50 DEG C, enzyme concentration is 800U/g substrates, pH is 9, digests 12h, take out 80
DEG C hot water in keep the temperature 60min, the fibroin slurries after being inactivated, by Cellulose nanocrystal must be added to inactivation after fibroin starch
Copy paper is carried out in liquid, obtains silk paper.Wherein Cellulose nanocrystal must account for the 8% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Embodiment 3
A kind of silk mask of containing cellulose nano whisker, preparation method are as follows：
(1) silk raw material is added in 100 DEG C of water, is handled as 3h, the mass ratio of silk and deionized water is 1:50, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 90 DEG C, mass fraction is 5%2CO3In solution, after reacting 40min, with 90 DEG C go
Ionized water is cleaned, and puts into 90 DEG C again, the Na that mass fraction is 5%2CO3In solution, 40min is reacted, is repeated 10 times, it will
The fibroin fiber of acquisition is cleaned to neutrality；Wherein the mass ratio of silk and sodium carbonate is 100:5.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), are 1000r/min in rotating speed
Under be dispersed with stirring uniformly, and under conditions of temperature is 70 DEG C, enzyme concentration is 1500U/g substrates, pH is 8, digest 8h, take out and exist
60min is kept the temperature in 80 DEG C of hot water, Cellulose nanocrystal must be added to the fibroin after inactivation by the fibroin slurries after being inactivated
Copy paper is carried out in slurries, obtains silk paper.Wherein Cellulose nanocrystal must account for the 20% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Embodiment 4
A kind of silk mask of containing cellulose nano whisker, preparation method are as follows：
(1) silk raw material is added in 100 DEG C of water, is handled as 2h, the mass ratio of silk and deionized water is 1:20, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 80 DEG C, mass fraction is 0.8%2CO3In solution, after reacting 45min, with 80 DEG C
Deionized water is cleaned, and puts into 80 DEG C again, the Na that mass fraction is 0.8%2CO3In solution, 30min is reacted, is repeated 8 times,
The fibroin fiber of acquisition is cleaned to neutrality；Wherein the mass ratio of silk and sodium carbonate is 100:3.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 100r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 70 DEG C, enzyme concentration is 1200U/g substrates, pH is 7, digests 8h, take out 80
DEG C hot water in keep the temperature 30min, the fibroin slurries after being inactivated, by Cellulose nanocrystal must be added to inactivation after fibroin starch
Copy paper is carried out in liquid, obtains silk paper.Wherein Cellulose nanocrystal must account for the 12% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Embodiment 5
A kind of silk mask of containing cellulose nano whisker, preparation method are as follows：
(1) silk raw material is added in 100 DEG C of water, is handled as 3h, the mass ratio of silk and deionized water is 1:10, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 90 DEG C, mass fraction is 2%2CO3In solution, after reacting 45min, with 90 DEG C go
Ionized water is cleaned, and puts into 90 DEG C again, the Na that mass fraction is 2%2CO3In solution, 45min is reacted, repeats 6 times, will obtain
The fibroin fiber obtained is cleaned to neutrality；Wherein the mass ratio of silk and sodium carbonate is 100:4.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 400r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 60 DEG C, enzyme concentration is 1000U/g substrates, pH is 7, digests 4h, take out 90
DEG C hot water in keep the temperature 20min, the fibroin slurries after being inactivated, by Cellulose nanocrystal must be added to inactivation after fibroin starch
Copy paper is carried out in liquid, obtains silk paper.Wherein Cellulose nanocrystal must account for the 10% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Embodiment 6
A kind of silk mask of containing cellulose nano whisker, preparation method are as follows：
(1) silk raw material is added in 100 DEG C of water, is handled as 2h, the mass ratio of silk and deionized water is 1:5, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 80 DEG C, mass fraction is 1%2CO3In solution, after reacting 45min, with 80 DEG C go
Ionized water is cleaned, and puts into 80 DEG C again, the Na that mass fraction is 1%2CO3In solution, 45min is reacted, repeats 4 times, will obtain
The fibroin fiber obtained is cleaned to neutrality；Wherein the mass ratio of silk and sodium carbonate is 100:5.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 600r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 60 DEG C, enzyme concentration is 1000U/g substrates, pH is 7, digests 4h, take out 90
DEG C hot water in keep the temperature 30min, the fibroin slurries after being inactivated, by Cellulose nanocrystal must be added to inactivation after fibroin starch
Copy paper is carried out in liquid, obtains silk paper.Wherein Cellulose nanocrystal must account for the 16% of fibroin grind slurries quality.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Comparative example 1
A kind of silk mask for the Cellulose nanocrystal palpus that undopes, preparation method are as follows：
(1) silk raw material is added in 95 DEG C of water, is handled as 1h, the mass ratio of silk and deionized water is 1:1, centrifugation
Alkali process is carried out after dehydration.The centrifugation is carried out using flat centrifuge, and the condition of centrifugation is：Rotating speed is 3000rpm,
Centrifugation time is 15min.The alkali process is specially：By the Na that silk is immersed in 80 DEG C, mass fraction is 0.1%2CO3It is molten
It in liquid, after reacting 30min, is cleaned with 80 DEG C of deionized waters, puts into 80 DEG C again, the Na that mass fraction is 0.1%2CO3Solution
In, 30min is reacted, repeats 1 time, the fibroin fiber of acquisition is cleaned to neutrality；The wherein matter of silk and sodium carbonate
Amount is than being 100:1.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 800r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 50 DEG C, enzyme concentration is 800U/g substrates, pH is 6, digests 6h, take out 80
DEG C hot water in keep the temperature 10min, the fibroin slurries after being inactivated.Copy paper will be carried out in the fibroin slurries after inactivation again, obtained
Silk paper.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Comparative example 2
A kind of silk mask for the Cellulose nanocrystal palpus that undopes, preparation method are as follows：
(1) silk raw material is added in 95 DEG C of water, is handled as 3h, the mass ratio of silk and deionized water is 1:100, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 85 DEG C, mass fraction is 10%2CO3In solution, after reacting 60min, with 85 DEG C
Deionized water is cleaned, and puts into 85 DEG C again, the Na that mass fraction is 10%2CO3In solution, 60min is reacted, is repeated 5 times,
The fibroin fiber of acquisition is cleaned to neutrality.Wherein the mass ratio of silk and sodium carbonate is 100:10.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 400r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 50 DEG C, enzyme concentration is 1200U/g substrates, pH is 9, digests 12h, take out
60min is kept the temperature in 80 DEG C of hot water, the fibroin slurries after being inactivated.Copy paper will be carried out in the fibroin slurries after inactivation again, obtained
To silk paper.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Comparative example 3
A kind of silk mask for the Cellulose nanocrystal palpus that undopes, preparation method are as follows：
(1) silk raw material is added in 100 DEG C of water, is handled as 2h, the mass ratio of silk and deionized water is 1:20, from
Alkali process is carried out after heart dehydration.The condition of the centrifugation is：Rotating speed is 3000rpm, centrifugation time 15min.The alkali
Processing is specially：By the Na that silk is immersed in 80 DEG C, mass fraction is 0.8%2CO3In solution, after reacting 45min, with 80 DEG C
Deionized water is cleaned, and puts into 80 DEG C again, the Na that mass fraction is 0.8%2CO3In solution, 30min is reacted, is repeated 8 times,
The fibroin fiber of acquisition is cleaned to neutrality；Wherein the mass ratio of silk and sodium carbonate is 100:5.
(2) Alealase2.4L enzymes are mixed into the fibroin fiber obtained in step (1), in the case where rotating speed is 200r/min
It is dispersed with stirring uniformly, and under conditions of temperature is 70 DEG C, enzyme concentration is 1000U/g substrates, pH is 7, digests 8h, take out 80
DEG C hot water in keep the temperature 30min, the fibroin slurries after being inactivated.Copy paper will be carried out in the fibroin slurries after inactivation again, obtained
Silk paper.
(3) silk paper obtained in step (2) is immersed in 25g Essences, then sterilizes, seals, packaging, obtains silkworm
Silk mask product.
Effect example
(1) moisturizing degree is evaluated
The silk mask obtained by Examples 1 to 6 and comparative example 1~3 is cut by the circle of a diameter of 20mm sizes, and
After measuring its initial weight, be affixed to 30 healthy all ages and classes, gender and the personnel that have cosmetic base it is upper
It on the inside of arm and maintains 30 minutes, its weight is then removed and measure, to calculate its difference.Moisture evaporation in order to prevent, to it
Cover the same plastics of size and fixation.
It is using the device measured to percutaneous moisture loss amount (Transepidermal water loss)
Tewarmeter TM210 (Courage and khazaka companies, Germany) measure moisture loss amount (g/m2h)。
Said determination is carried out respectively to 30, finds out the worth average value obtained from them, its knot is shown from the following table 1
Fruit.
The evaluation of 1 moisturizing degree of table
Shown in upper table 1, when the embodiment of the present invention 1~6 is compared with reference examples 1~3, showed through subcutaneously losing
Significantly low measured value, it may be determined that compared with the silk mask for using the Cellulose nanocrystal palpus that undopes, received doped with cellulose
The silk mask skin moisture-keeping power of meter Jing Xu is more superior.
(2) metrics evaluation
Experimental method：Items of the personnel to cosmetics for having cosmetic base knowledge of 30 all ages and classes of selection, gender
Index scores item by item.
Set evaluation index：Moisturizing, whitening, anti-wrinkle, anti-acne, moisturizing.
Setting evaluation performance rate：Excessively poor (1~2), very poor (3~4), general (5~6), preferably (7~8), fabulous (9
~10).
Silk mask synthetic user in Examples 1 to 6 doped with Cellulose nanocrystal palpus is evaluated：30 sensory evaluation people
Member is divided situation as shown in table 2 facial mask indices.
2 30 sensory evaluation personnel of table are to facial mask indices to a point evaluation
Silk mask synthetic user is evaluated in comparative example 1~3：30 sensory evaluation personnel are divided feelings to facial mask indices
Condition is as shown in table 3.
3 30 sensory evaluation personnel of table are to facial mask indices to a point evaluation
The characteristics of large specific surface area using Cellulose nanocrystal palpus, strong adsorption being can be seen that from table 2, the comparison of table 3,
In terms of moisturizing, whitening, anti-wrinkle, more there is superiority doped with the silk mask of Cellulose nanocrystal palpus.Therefore, the present invention is utilized
Method prepare silk mask have efficient whitening, anti-wrinkle and moisturizing performance, can more meet the demand in market.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the silk paper of doping Cellulose nanocrystal palpus, which is characterized in that include the following steps：
(1) centrifugation removes moisture after silk being carried out hot-water pretreatment, then carries out alkali process, then clean to neutrality, obtains silk
Cellulose fiber；
(2) protease is added in the fibroin fiber obtained in step (1), is digested after being uniformly mixed, then by enzyme
The fibroin slurries obtained after solution carry out inactivation treatment, the fibroin slurries after being inactivated；
(3) Cellulose nanocrystal must be added in the fibroin slurries after the inactivation obtained in step (2) and carries out copy paper, be mixed
The silk paper of miscellaneous Cellulose nanocrystal palpus.
2. the preparation method of the silk paper of doping Cellulose nanocrystal palpus according to claim 1, it is characterised in that：
The mass ratio of silk and water described in step (1) is 1:(1~100)；
The additive amount of protease described in step (2) is pressed to be calculated per g fibroin fiber proportioning 500~1500U protease；
The additive amount of Cellulose nanocrystal palpus described in step (3) must be accounted for the 4% of fibroin grind slurries quality by Cellulose nanocrystal
~20% calculates.
3. the preparation method of the silk paper of doping Cellulose nanocrystal palpus according to claim 1, it is characterised in that：
Protease described in step (2) is Alealase 2.4L enzymes, papain, trypsase and Havorzyme albumen
It is one or more of in enzyme.
4. the preparation method of the silk paper of doping Cellulose nanocrystal palpus according to claim 1, which is characterized in that
The condition of hot-water pretreatment described in step (1) is：1~3h is handled in 95~100 DEG C of hot water；
Alkali process described in step (1) is achieved by the steps of：Silk is immersed in 80~100 DEG C, mass fraction 0.1
~10% Na2CO330~60min is reacted in solution, then uses 80~100 DEG C of water clean, put into 80 again~
100 DEG C, the Na that mass fraction is 0.1~10%2CO330~60min, repetitive operation 1~10 time are reacted in solution；
The condition of enzymolysis described in step (2) is：4~12h is digested under conditions of pH is 6~9, temperature is 50~70 DEG C；
The condition of inactivation treatment described in step (2) is：10~60min is kept the temperature in 80~100 DEG C of hot water.
5. a kind of silk paper of doping Cellulose nanocrystal palpus, it is characterised in that：Pass through Claims 1 to 4 any one of them
Method is prepared.
6. application of the silk paper of the doping Cellulose nanocrystal palpus described in claim 5 in cosmetic field.
7. a kind of silk mask of doping Cellulose nanocrystal palpus, it is characterised in that：By the way that the doping described in claim 5 is fine
The silk paper of the plain nano whisker of dimension, which is impregnated into Essence, to be obtained.
8. the silk mask of doping Cellulose nanocrystal palpus according to claim 7, it is characterised in that：The Essence
To include the essence of aloe extract, purslane extract, yeast extract, glycine betaine, sodium alginate and royal jelly extract
Liquid.
9. the silk mask of doping Cellulose nanocrystal palpus according to claim 8, which is characterized in that the Essence
It includes the component counted in parts by weight as follows to be：60 parts of water, 12 parts of glycerine, 8 parts of polyethylene glycol, 0.2 part of Sodium Hyaluronate, water
Solve 0.4 part of collagen, 8 parts of aloe extract, 3 parts of purslane extract, 4 parts of yeast extract, 4 parts of glycine betaine, sodium alginate 2
Part, 3 parts of royal jelly extract, 0.2 part of Phenoxyethanol.
10. claim 7~9 any one of them adulterate Cellulose nanocrystal must silk mask cosmetics moisturizing, whitening,
And/or it is applied in anti-wrinkle field.
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