CN103340770B - Preparation method for hair dye based on walnut green husk pigment - Google Patents
Preparation method for hair dye based on walnut green husk pigment Download PDFInfo
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Abstract
The invention relates to a preparation method of a hair dye, especially to a preparation method for a botanical hair dye, and specifically relates to a preparation method for a hair dye based on a walnut green husk pigment. The preparation method comprises the following steps: striping walnut green husk, air drying in a shady place; crushing, sieving through a sieve of 70-90 meshes; adding green husk powder and acetone into a container with a solid-liquid mass ratio of 1:25-35 and an acetone concentration of 70-90%, oscillation processing the solution at a constant temperature of 40-50 DEG C for 10-14 h; centrifuging the solution for 2-4 times, filtering off impurities and collecting the supernatant; decompressing concentrating the solution at a temperature of 50-65 DEG C to obtain an ointment; and preparing the hair dye according to the following material ratios: 5-7% of the ointment, 85-87% of water, 0.5-1.5% of silicone oil, 0.5-1.5% of oil-solubility VE, 0.5-1.5% of VB, 3-5% of olive oil and 0.5-1.5% of white vaseline. The preparation method is simple, easy to operate and high in recovery rate. The prepared green husk pigment is granular, shows yellow under the developing effect of methyl red, has no escherichia coli, is suitable for exploitation of the hair dye, and helps to solve the problems that the conventional hair dye contains carcinogenesis substances and the natural hair dye is not exploited fully.
Description
Technical field
The present invention relates to the preparation method of hair dye, particularly relate to the preparation method of plant source hair dye, be specially a kind of hair dye preparation method based on walnut green husk pigment.
Background technology
Semen Juglandis belongs to Juglandaceae Juglans, formal name used at school Semen Juglandis (
juglans regia L.), China's Semen Juglandis cultivated area reaches 3,175 ten thousand mu, and nearly 500,000 tons of annual production, total cultivated area, annual production and Pericarpium Citri Reticulatae Viride garbage all rank first in the world.Containing the Pericarpium Citri Reticulatae Viride such as purpurin and marennin pigment in Exocarpium Juglandis Immaturus, time immemorial just useful Exocarpium Juglandis Immaturus to dye cloth the record of material, Pericarpium Citri Reticulatae Viride pigment also exists for the fact contaminating head.Current hair dye has become product with fastest developing speed, the most powerful in hair care industry, present stage, China became hair dye production and selling big country in the world, according to expert expects, in 5 years from now on, the growth rate of China's hair dyeing population will far away higher than global average level, and the market development of hair dye has a extensive future.But due to flooding the market of defective cosmetics, as detect in traditional hair dye can be carcinogenic banned substance 2,4-diamino anisole and o-phenylenediamine, these harmful substances have caused the impaired accident of a lot of consumers body and mind, all there is report both at home and abroad, therefore the natural hair dye of development of new more and more comes into one's own, and also has boundless application prospect simultaneously.
Summary of the invention
The present invention contains the problem of carcinogen and natural hair dye underexploitation in order to solve traditional hair dye, provide a kind of hair dye preparation method based on walnut green husk pigment.
The present invention adopts following technical scheme to realize: the first preparation method of a kind of hair dye based on walnut green husk pigment, comprises the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
After pulverizing, 70-90 eye mesh screen sieves;
Add Pericarpium Citri Reticulatae Viride powder and acetone in a reservoir in the ratio of solid-liquid mass ratio 1:25-35, the concentration of acetone is 70-90%, and solution is oscillation treatment 10-14h at constant temperature 40-50 DEG C;
Above-mentioned solution centrifugal process 2-4 time, filter is assorted collects supernatant;
Supernatant concentrating under reduced pressure at 55-65 DEG C of temperature obtains ointment;
By ointment 5-7%, water 85-87%, silicone oil 0.5-1.5%, oil-soluble V
e0.5-1.5%, V
bthe part by weight of 0.5-1.5%, olive oil 3-5%, white vaseline 0.5-1.5% is mixed with hair dye.
The invention provides a kind of method producing natural hair dye, first Exocarpium Juglandis Immaturus is dried in shady spot, in shady spot, oxidation reaction is less likely to occur Exocarpium Juglandis Immaturus, active substance in Pericarpium Citri Reticulatae Viride is not easy to vapor away, Pericarpium Citri Reticulatae Viride dries rear pulverizing, sieve with 70-90 eye mesh screen, the most cell structure damage of Pericarpium Citri Reticulatae Viride powder after the screen cloth of this kind of specification sieves, the blue or green skin pigment damaging cell and discharge can be dissolved with the mixed acetone of Pericarpium Citri Reticulatae Viride powder, and concentration to be the acetone solution of 70-90% effective, at constant temperature 40-50 DEG C, oscillation treatment can accelerate the dissolving of Pericarpium Citri Reticulatae Viride pigment, the character that acetone can dissolve Pericarpium Citri Reticulatae Viride pigment is drawn through test of many times by scientific research personnel, paid performing creative labour for this reason, the cell wall constituent such as pectin, cellulose in Exocarpium Juglandis Immaturus cell can be got rid of by centrifugal treating, and these become branch to affect the spilling of Pericarpium Citri Reticulatae Viride pigment, get rid of the purity that these compositions also can improve Pericarpium Citri Reticulatae Viride element, solution after purification finally at 55-65 DEG C of temperature concentrating under reduced pressure obtain ointment, in this temperature range, acetone is volatile, acetone can and the Pericarpium Citri Reticulatae Viride pigment separated that will obtain, and don't destroy the activity of Pericarpium Citri Reticulatae Viride pigment, last by the Pericarpium Citri Reticulatae Viride pigment ointment obtained and water, silicone oil, oil-soluble V
e, V
b, olive oil, white vaseline obtained hair dye in proportion, added olive oil contains vitamin B and E, makes hair fully absorb nutrient.
Based on the second preparation method of the hair dye of walnut green husk pigment, further comprising the steps of: the centrifugal supernatant obtained repeatedly added the ethanol the floccule of filtering appearance that concentration is 80-95% before concentrating under reduced pressure, till occurring without floccule.
The alcohols energy added in supernatant and the reaction such as protein, pectin generate precipitate or floccule, improve the purity of Pericarpium Citri Reticulatae Viride pigment.
Based on the third preparation method of the hair dye of walnut green husk pigment, further comprising the steps of: to be first placed in container by before the Exocarpium Juglandis Immaturus powder after sieving and acetone mixing, to add pure water in the ratio of solid-liquid mass ratio 1:8-12; In above-mentioned solution, add concentration is that 1-2.5g/L is with pectase and the cellulase arbitrarily than mixing, add with the ratio of the volume ratio 1:90-110 of enzyme and solution, the ph value of solution is adjusted to by seal of vessel after 5.5-6.7, oscillation treatment 36-60h under 30-50 DEG C of constant temperature; When adding acetone, add with the ratio that the volume ratio of acetone and enzymolysis solution is 1:12-18.
Pericarpium Citri Reticulatae Viride powder and pure water take mass ratio as the ratio mixing of 1:8-12, and make Pericarpium Citri Reticulatae Viride powder easily by enzymolysis, Pericarpium Citri Reticulatae Viride powder is mixed with solution and have selected pure water, and the ion in pure water is few, little on the enzymolysis impact of Pericarpium Citri Reticulatae Viride powder, the pectase added in the solution decomposes Exocarpium Juglandis Immaturus cell intercellular layer and primary wall, and natural pectin is decomposed completely, destroys cell wall structure, to reach the object of isolated cell, utilize the cellulosic molecule in cellulase decomposition primary wall and secondary wall, promote the release of various chemically reactive substance in cell, and concentration be 1-2.5g/L pectase and cellulase can thorough fast must by Exocarpium Juglandis Immaturus enzymolysis, and the ph of solution is transferred to 5.5-6.7, and react under 30-50 DEG C of constant temperature, the activity of pectase and cellulase is maximum, be beneficial to the enzymolysis of Exocarpium Juglandis Immaturus, the enzymolysis of the present invention to Exocarpium Juglandis Immaturus is the cellularity destroying Exocarpium Juglandis Immaturus further, improve the extraction ratio of Pericarpium Citri Reticulatae Viride pigment, and during enzymolysis, selected pectase and cellulase, it is a kind of biological method, can not destroy again the activity of Pericarpium Citri Reticulatae Viride pigment by chemically reactive substance in release cells.
A kind of 4th kind of preparation method of the hair dye based on walnut green husk pigment, further comprising the steps of: the solution after enzymolysis is prepended on microwave ultrasonic extraction instrument what add acetone, microwave power is set to 100-250W, ultrasonic frequency is set to 20-30KHz, ultrasonic power is set to 900-1200W, and the time is 20-36min.
The microwave and ultrasound process of solution after enzymolysis is the enzymolysis of assisting Exocarpium Juglandis Immaturus with physical method, by thorough enzymolysis, and the release that the Pericarpium Citri Reticulatae Viride pigment in cell is tried one's best, thus the extraction ratio improving Pericarpium Citri Reticulatae Viride pigment.
The inventive method is simple, be easy to operation, reagent is recyclable, pollution-free, and environmental protection, extraction ratio is high; Obtained Pericarpium Citri Reticulatae Viride pigment is graininess, tasteless, soluble in water, all stable to light, heat, oxidant, reducing agent, VitAVitE, cysteine, through C.I. 13020. colour developing in yellow, without escherichia coli, be applicable to hair dye exploitation, and obtained plant source hair dye, no side effects is a kind of high-quality natural pigment preferably; This method is raw materials used to be easy to get, cheap; Present stage, hair dye became product with fastest developing speed, the most powerful in hair care industry, and China has become hair dye production and selling big country in the world, and the market development of plant source hair dye has a extensive future.
Detailed description of the invention
Embodiment one:
Based on a hair dye preparation method for walnut green husk pigment, comprise the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
70(or 80 or 90 after pulverizing) eye mesh screen sieves;
In solid-liquid mass ratio 1:25(or 28 or 30 or 32 or 35) ratio add Pericarpium Citri Reticulatae Viride powder and acetone in a reservoir, the concentration of acetone is 70(or 75 or 80 or 85 or 90) %, solution is at constant temperature 40(or 42 or 45 or 48 or 50) DEG C at oscillation treatment 10(or 11 or 12 or 13 or 14) h;
Add the solution centrifugal process 2(or 3 or 4 after acetone) secondary, filter is assorted collects supernatant;
By supernatant at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment at DEG C temperature;
By ointment 5(or 6 or 7) %, water 85(or 86 or 87) %, silicone oil 1.5(or 1 or 0.5) %, oil-soluble V
e1.5(or 1 or 0.5) %, V
b0.5(or 1 or 1.5) %, olive oil 5(or 4 or 3) %, white vaseline 1.5(or 1 or 0.5) part by weight of % is mixed with hair dye.
Embodiment two:
Based on a hair dye preparation method for walnut green husk pigment, comprise the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
70(or 80 or 90 after pulverizing) eye mesh screen sieves;
In solid-liquid mass ratio 1:25(or 28 or 30 or 32 or 35) ratio add Pericarpium Citri Reticulatae Viride powder and acetone in a reservoir, the concentration of acetone is 70(or 75 or 80 or 85 or 90) %, solution is at constant temperature 40(or 42 or 45 or 48 or 50) DEG C at oscillation treatment 10(or 11 or 12 or 13 or 14) h;
Add the solution centrifugal process 2(or 3 or 4 after acetone) secondary, filter is assorted collects supernatant;
In supernatant, repeatedly add concentration is 80(or 84 or 87 or 91 or 95) floccule that occurs of the ethanol of % filtering, till occurring without floccule;
To the solution after ethanol be added at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment at DEG C temperature;
By ointment 5(or 6 or 7) %, water 85(or 86 or 87) %, silicone oil 1.5(or 1 or 0.5) %, oil-soluble V
e1.5(or 1 or 0.5) %, V
b0.5(or 1 or 1.5) %, olive oil 5(or 4 or 3) %, white vaseline 1.5(or 1 or 0.5) part by weight of % is mixed with hair dye.
Embodiment three:
Based on a hair dye preparation method for walnut green husk pigment, comprise the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
70(or 80 or 90 after pulverizing) eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed in container, in solid-liquid mass ratio 1:8(or 10 or 12) ratio add pure water;
Adding concentration is in a reservoir 1(or 1.5 or 2 or 2.5) g/L with arbitrarily than mixing pectase and cellulase, volume ratio 1:90(or 95 or 100 or 105 or 110 with enzyme and solution) ratio add, solution ph is adjusted to 5.5(or 6 or 6.7) after by seal of vessel, at 30(or 35 or 40 or 45 or 50) oscillation treatment 36(or 42 or 48 or 54 or 60 under DEG C constant temperature) h;
Adding concentration in solution after enzymolysis is 70(or 75 or 80 or 85 or 90)) acetone of %, with the volume ratio of acetone and enzymolysis solution for 1:12(or 14 or 16 or 18) ratio add, solution is at constant temperature 40(or 42 or 45 or 48 or 50) DEG C at oscillation treatment 10(or 11 or 12 or 13 or 14) h;
Add solution centrifugal process 2(or 3 or 4 after acetone) secondary, filter is assorted collects supernatant;
In supernatant, repeatedly add concentration is 80(or 84 or 87 or 91 or 95) floccule that occurs of the ethanol of % filtering, till occurring without floccule;
To the solution after ethanol be added at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment at DEG C temperature;
By ointment 5(or 6 or 7) %, water 85(or 86 or 87) %, silicone oil 1.5(or 1 or 0.5) %, oil-soluble V
e1.5(or 1 or 0.5) %, V
b0.5(or 1 or 1.5) %, olive oil 5(or 4 or 3) %, white vaseline 1.5(or 1 or 0.5) part by weight of % is mixed with hair dye.
Embodiment four:
Based on a hair dye preparation method for walnut green husk pigment, comprise the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
70(or 80 or 90 after pulverizing) eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed in container, in solid-liquid mass ratio 1:8(or 10 or 12) ratio add pure water;
Adding concentration is in a reservoir 1(or 1.5 or 2 or 2.5) g/L with arbitrarily than mixing pectase and cellulase, volume ratio 1:90(or 95 or 100 or 105 or 110 with enzyme and solution) ratio add, solution ph is adjusted to 5.5(or 6 or 6.7) after by seal of vessel, at 30(or 35 or 40 or 45 or 50) oscillation treatment 36(or 42 or 48 or 54 or 60 under DEG C constant temperature) h;
Solution after enzymolysis is placed on microwave ultrasonic extraction instrument, microwave power is set to 100(or 150 or 200 or 250) W, ultrasonic frequency is set to 20(or 22 or 24 or 26 or 28 or 30) KHz, ultrasonic power is set to 900(or 1000 or 1100 or 1200) W, the time is 20(or 24 or 28 or 32 or 36) min;
Adding concentration in solution after microwave ultrasonic wave process is 70(or 75 or 80 or 85 or 90)) acetone of %, with the volume ratio of acetone and enzymolysis solution for 1:12(or 14 or 16 or 18) ratio add, solution is at constant temperature 40(or 42 or 45 or 48 or 50) DEG C at oscillation treatment 10(or 11 or 12 or 13 or 14) h;
Add the solution centrifugal process 2(or 3 or 4 after acetone) secondary, filter is assorted collects supernatant;
In supernatant, repeatedly add concentration is 80(or 84 or 87 or 91 or 95) floccule that occurs of the ethanol of % filtering, till occurring without floccule;
To the solution after ethanol be added at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment at DEG C temperature;
By ointment 5(or 6 or 7) %, water 85(or 86 or 87) %, silicone oil 1.5(or 1 or 0.5) %, oil-soluble V
e1.5(or 1 or 0.5) %, V
b0.5(or 1 or 1.5) %, olive oil 5(or 4 or 3) %, white vaseline 1.5(or 1 or 0.5) part by weight of % is mixed with hair dye.
Claims (4)
1., based on a hair dye preparation method for walnut green husk pigment, it is characterized in that comprising the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
After pulverizing, 70-90 eye mesh screen sieves;
Add Pericarpium Citri Reticulatae Viride powder and acetone in a reservoir in the ratio of solid-liquid mass ratio 1:25-35, the concentration of acetone is 70-90%, and solution is oscillation treatment 10-14h at constant temperature 40-50 DEG C;
Above-mentioned solution centrifugal process 2-4 time, filter is assorted collects supernatant;
Supernatant concentrating under reduced pressure at 55-65 DEG C of temperature obtains ointment;
By ointment 5-7%, water 85-87%, silicone oil 0.5-1.5%, oil-soluble V
e0.5-1.5%, V
bthe part by weight of 0.5-1.5%, olive oil 3-5%, white vaseline 0.5-1.5% is mixed with hair dye.
2., based on a hair dye preparation method for walnut green husk pigment, it is characterized in that comprising the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
After pulverizing, 70-90 eye mesh screen sieves;
Add Pericarpium Citri Reticulatae Viride powder and acetone in a reservoir in the ratio of solid-liquid mass ratio 1:25-35, the concentration of acetone is 70-90%, and solution is oscillation treatment 10-14h at constant temperature 40-50 DEG C;
Above-mentioned solution centrifugal process 2-4 time, filter is assorted collects supernatant;
Ethanol the floccule of filtering appearance that concentration is 80-95% is repeatedly added, till occurring without floccule in supernatant;
Ointment is obtained by adding the concentrating under reduced pressure at 55-65 DEG C of temperature of the solution after ethanol;
By ointment 5-7%, water 85-87%, silicone oil 0.5-1.5%, oil-soluble V
e0.5-1.5%, V
bthe part by weight of 0.5-1.5%, olive oil 3-5%, white vaseline 0.5-1.5% is mixed with hair dye.
3., based on a hair dye preparation method for walnut green husk pigment, it is characterized in that comprising the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
After pulverizing, 70-90 eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed in container, adds pure water in the ratio of solid-liquid mass ratio 1:8-12;
In above-mentioned solution, add concentration is that 1-2.5g/L is with pectase and the cellulase arbitrarily than mixing, add with the ratio of the volume ratio 1:90-110 of enzyme and solution, the ph value of solution is adjusted to by seal of vessel after 5.5-6.7, oscillation treatment 36-60h under 30-50 DEG C of constant temperature;
Add the acetone that concentration is 70-90% in solution after enzymolysis, add with the ratio that the volume ratio of acetone and enzymolysis solution is 1:12-18, solution is oscillation treatment 10-14h at constant temperature 40-50 DEG C;
Add solution centrifugal process after acetone 2-4 time, filter is assorted collects supernatant;
Ethanol the floccule of filtering appearance that concentration is 80-95% is repeatedly added, till occurring without floccule in supernatant;
Ointment is obtained by adding the concentrating under reduced pressure at 55-65 DEG C of temperature of the solution after ethanol;
By ointment 5-7%, water 85-87%, silicone oil 0.5-1.5%, oil-soluble V
e0.5-1.5%, V
bthe part by weight of 0.5-1.5%, olive oil 3-5%, white vaseline 0.5-1.5% is mixed with hair dye.
4., based on a hair dye preparation method for walnut green husk pigment, it is characterized in that comprising the following steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
After pulverizing, 70-90 eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed in container, adds pure water in the ratio of solid-liquid mass ratio 1:8-12;
In above-mentioned solution, add concentration is that 1-2.5g/L is with pectase and the cellulase arbitrarily than mixing, add with the ratio of the volume ratio 1:90-110 of enzyme and solution, the ph value of solution is adjusted to by seal of vessel after 5.5-6.7, oscillation treatment 36-60h under 30-50 DEG C of constant temperature;
Solution after enzymolysis is placed on microwave ultrasonic extraction instrument, and microwave power is set to 100-250W, and ultrasonic frequency is set to 20-30KHz, and ultrasonic power is set to 900-1200W, and the time is 20-36min;
Add the acetone that concentration is 70-90% in solution after enzymolysis, add with the ratio that the volume ratio of acetone and enzymolysis solution is 1:12-18, solution is oscillation treatment 10-14h at constant temperature 40-50 DEG C;
Add solution centrifugal process after acetone 2-4 time, filter is assorted collects supernatant;
In supernatant, repeatedly add alcohols material the floccule of filtering appearance that concentration is 80-95%, add alcohols material till occurring without floccule;
Ointment is obtained by adding the concentrating under reduced pressure at 55-65 DEG C of temperature of the solution after ethanol;
By ointment 5-7%, water 85-87%, silicone oil 0.5-1.5%, oil-soluble V
e0.5-1.5%, V
bthe part by weight of 0.5-1.5%, olive oil 3-5%, white vaseline 0.5-1.5% is mixed with hair dye.
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