CN103340770A - Preparation method for hair dye based on walnut green husk pigment - Google Patents
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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, relate in particular to the preparation method of plant source hair dye, be specially a kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment.
Background technology
Semen Juglandis belongs to the Juglandaceae Juglans, the formal name used at school Semen Juglandis (
Juglans regia L.), China's Semen Juglandis cultivated area reaches 3,175 ten thousand mu, nearly 500,000 tons of annual production, and total cultivated area, annual production and Pericarpium Citri Reticulatae Viride garbage all rank first in the world.Contain Pericarpium Citri Reticulatae Viride pigments such as purpurin and marennin in the Exocarpium Juglandis Immaturus, the record of dying cloth and expecting with regard to useful Exocarpium Juglandis Immaturus in time immemorial, the Pericarpium Citri Reticulatae Viride pigment also exists for the fact of dying head.Hair dye has become with fastest developing speed, the most powerful product in the hair care industry at present, present stage, China became hair dye production and selling big country in the world, estimate according to the expert, in 5 years from now on, China's hair dyeing Increase of population speed will be higher than global average level far away, and the market development of hair dye has a extensive future.But owing to flooding the market of defective cosmetics, as in traditional hair dye, detect 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, report is all arranged both at home and abroad, therefore develop novel natural hair dye and more and more come into one's own, also have boundless application prospect simultaneously.
Summary of the invention
The present invention provides a kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment in order to solve the problem that traditional hair dye contains carcinogen and natural hair dye underexploitation.
The present invention adopts following technical scheme to realize: a kind of first kind of preparation method of the hair dye based on the Exocarpium Juglandis Immaturus pigment may further comprise the steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
Pulverizing back 70-90 eye mesh screen sieves;
Ratio in solid-liquid mass ratio 1:25-35 adds Pericarpium Citri Reticulatae Viride powder and acetone in container, the concentration of acetone is 70-90%, and solution is at constant temperature 40-50 ℃ of following oscillation treatment 10-14h;
Above-mentioned solution centrifugal is handled 2-4 time, the assorted supernatant of collecting of filter;
Supernatant concentrating under reduced pressure under 55-65 ℃ of temperature obtains ointment;
Press 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 of producing natural hair dye, earlier Exocarpium Juglandis Immaturus is dried in shady spot, be not easy to take place oxidation reaction at shady spot's Exocarpium Juglandis Immaturus, active substance in the Pericarpium Citri Reticulatae Viride is not easy to vapor away, Pericarpium Citri Reticulatae Viride dries the back and pulverizes, sieve with the 70-90 eye mesh screen, the most cell structure damage of Pericarpium Citri Reticulatae Viride powder after the screen cloth of this kind specification sieves, can dissolve the Pericarpium Citri Reticulatae Viride pigment that the damage cell discharges with the mixed acetone of Pericarpium Citri Reticulatae Viride powder, and concentration is that the acetone solution of 70-90% is effective, can accelerate the dissolving of Pericarpium Citri Reticulatae Viride pigment constant temperature 40-50 ℃ of following oscillation treatment, the character that acetone can dissolve the Pericarpium Citri Reticulatae Viride pigment is drawn through test of many times by the scientific research personnel, has paid performing creative labour for this reason; Centrifugal treating can be got rid of cell wall constituents such as pectin, cellulose in the Exocarpium Juglandis Immaturus cell, and these become branch to influence overflowing of Pericarpium Citri Reticulatae Viride pigment, get rid of the purity that these compositions also can improve the Pericarpium Citri Reticulatae Viride element; Solution after the purification at last under 55-65 ℃ of temperature concentrating under reduced pressure obtain ointment, under this temperature range, acetone is volatile, acetone can separate with the Pericarpium Citri Reticulatae Viride pigment that will make, and don't the activity of destruction Pericarpium Citri Reticulatae Viride pigment; At last by the Pericarpium Citri Reticulatae Viride pigment ointment that makes and water, silicone oil, oil-soluble V
E, V
B, olive oil, white vaseline make hair dye in proportion, added olive oil contains vitamin B and E, makes hair fully absorb nutrient.
A kind of second kind of preparation method of the hair dye based on the Exocarpium Juglandis Immaturus pigment, further comprising the steps of: the centrifugal supernatant that obtains repeatedly added the floccule that ethanol that concentration is 80-95% and filtering occur before concentrating under reduced pressure, till no floccule appearance.
The alcohols energy and the reactions such as protein, pectin that add in the supernatant generate precipitate or floccules, have improved the purity of Pericarpium Citri Reticulatae Viride pigment.
The third preparation method of a kind of hair dye based on the Exocarpium Juglandis Immaturus pigment, further comprising the steps of: as to place container before the Exocarpium Juglandis Immaturus powder after will sieving and acetone mix earlier, by the ratio adding pure water of solid-liquid mass ratio 1:8-12; Adding concentration in above-mentioned solution is that 1-2.5g/L is with any pectase and cellulase than mixing, ratio with the volume ratio 1:90-110 of enzyme and solution adds, the ph value of solution is transferred to behind the 5.5-6.7 with seal of vessel oscillation treatment 36-60h under 30-50 ℃ of constant temperature; When adding acetone, be that the ratio of 1:12-18 adds with the volume ratio of acetone and enzymolysis solution.
Pericarpium Citri Reticulatae Viride powder and pure water are that the ratio of 1:8-12 is mixed with the mass ratio, make the Pericarpium Citri Reticulatae Viride powder easily by enzymolysis, and the Pericarpium Citri Reticulatae Viride powder is mixed with solution and has selected pure water, and the ion in the pure water is few, and be little to the enzymolysis influence of Pericarpium Citri Reticulatae Viride powder; The pectase that adds in solution decomposes Exocarpium Juglandis Immaturus cell intercellular layer and primary wall, and natural pectin is decomposed fully, destroys cell wall structure, to reach the purpose of isolated cell; Utilize the cellulosic molecule in cellulase decomposition primary wall and the secondary wall, promote the release of various chemically reactive substances in the cell, and concentration be 1-2.5g/L pectase and cellulase can be thorough fast must be with the Exocarpium Juglandis Immaturus enzymolysis, and the ph of solution is transferred to 5.5-6.7, and under 30-50 ℃ of constant temperature, react, the active maximum of pectase and cellulase, be beneficial to the enzymolysis of Exocarpium Juglandis Immaturus, the present invention is the cellularity that further destroys Exocarpium Juglandis Immaturus to the enzymolysis of Exocarpium Juglandis Immaturus, improve the extraction ratio of Pericarpium Citri Reticulatae Viride pigment, and pectase and cellulase have been selected during enzymolysis for use, be a kind of biological method, can discharge the activity that chemically reactive substance in the cell does not destroy the Pericarpium Citri Reticulatae Viride pigment again.
A kind of the 4th kind of preparation method of the hair dye based on the Exocarpium Juglandis Immaturus pigment, further comprising the steps of: the solution behind the enzymolysis placed on the microwave ultrasonic wave extraction apparatus before adding acetone, microwave power is made as 100-250W, ultrasonic frequency is made as 20-30KHz, ultrasonic power is made as 900-1200W, and the time is 20-36min.
Solution behind the enzymolysis is the enzymolysis with the auxiliary Exocarpium Juglandis Immaturus of physical method with microwave and ultrasonic Treatment, with thorough enzymolysis, and the release that the Pericarpium Citri Reticulatae Viride pigment in the cell is tried one's best, thereby the extraction ratio of raising Pericarpium Citri Reticulatae Viride pigment.
The inventive method is simple, easy operating, reagent are recyclable, pollution-free, and environmental protection, the extraction ratio height; The Pericarpium Citri Reticulatae Viride pigment that makes is graininess, tasteless, soluble in water, all stable to light, heat, oxidant, Reducing agent, vitamin A, vitamin E, cysteine, be yellow through the C.I. 13020. colour developing, no escherichia coli, be fit to the hair dye exploitation, and the plant source hair dye that makes, no side effects is a kind of natural pigment of high-quality preferably; This method is raw materials used to be easy to get, cheap; Present stage, hair dye became with fastest developing speed, the most powerful product in the 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.
The specific embodiment
Embodiment one:
A kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment may further comprise the 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 in container, add Pericarpium Citri Reticulatae Viride powder and acetone, 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) ℃ following oscillation treatment 10(or 11 or 12 or 13 or 14) h;
The solution centrifugal that adds behind the acetone is handled 2(or 3 or 4) inferior, the assorted supernatant of collecting of filter;
With supernatant at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment under ℃ temperature;
Press 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:
A kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment may further comprise the 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 in container, add Pericarpium Citri Reticulatae Viride powder and acetone, 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) ℃ following oscillation treatment 10(or 11 or 12 or 13 or 14) h;
The solution centrifugal that adds behind the acetone is handled 2(or 3 or 4) inferior, the assorted supernatant of collecting of filter;
Repeatedly adding concentration in supernatant is 80(or 84 or 87 or 91 or 95) ethanol of % and the floccule that filtering occurs, till no floccule occurs;
To add solution behind the ethanol at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment under ℃ temperature;
Press 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:
A kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment may further comprise the 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 container, in solid-liquid mass ratio 1:8(or 10 or 12) ratio add pure water;
Adding concentration in container is 1(or 1.5 or 2 or 2.5) g/L with any than the pectase and the cellulase that mix, volume ratio 1:90(or 95 or 100 or 105 or 110 with enzyme and solution) ratio adds, solution ph is transferred to 5.5(or 6 or 6.7) after with 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 ℃ constant temperature) h;
Adding concentration in the solution behind enzymolysis is 70(or 75 or 80 or 85 or 90)) acetone of %, volume ratio with acetone and enzymolysis solution is 1:12(or 14 or 16 or 18) ratio add, solution is at constant temperature 40(or 42 or 45 or 48 or 50) ℃ following oscillation treatment 10(or 11 or 12 or 13 or 14) h;
Solution centrifugal is handled 2(or 3 or 4 after adding acetone) inferior, the assorted supernatant of collecting of filter;
Repeatedly adding concentration in supernatant is 80(or 84 or 87 or 91 or 95) ethanol of % and the floccule that filtering occurs, till no floccule occurs;
To add solution behind the ethanol at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment under ℃ temperature;
Press 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:
A kind of hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment may further comprise the 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 container, in solid-liquid mass ratio 1:8(or 10 or 12) ratio add pure water;
Adding concentration in container is 1(or 1.5 or 2 or 2.5) g/L with any than the pectase and the cellulase that mix, volume ratio 1:90(or 95 or 100 or 105 or 110 with enzyme and solution) ratio adds, solution ph is transferred to 5.5(or 6 or 6.7) after with 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 ℃ constant temperature) h;
Solution behind the enzymolysis places on the microwave ultrasonic wave extraction apparatus, microwave power is made as 100(or 150 or 200 or 250) W, ultrasonic frequency is made as 20(or 22 or 24 or 26 or 28 or 30) KHz, ultrasonic power is made as 900(or 1000 or 1100 or 1200) W, the time is 20(or 24 or 28 or 32 or 36) min;
Adding concentration in the solution after microwave ultrasonic wave is handled is 70(or 75 or 80 or 85 or 90)) acetone of %, volume ratio with acetone and enzymolysis solution is 1:12(or 14 or 16 or 18) ratio add, solution is at constant temperature 40(or 42 or 45 or 48 or 50) ℃ following oscillation treatment 10(or 11 or 12 or 13 or 14) h;
The solution centrifugal that adds behind the acetone is handled 2(or 3 or 4) inferior, the assorted supernatant of collecting of filter;
Repeatedly adding concentration in supernatant is 80(or 84 or 87 or 91 or 95) ethanol of % and the floccule that filtering occurs, till no floccule occurs;
To add solution behind the ethanol at 55(or 58 or 60 or 62 or 65) concentrating under reduced pressure obtains ointment under ℃ temperature;
Press 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. hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment is characterized in that may further comprise the steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
Pulverizing back 70-90 eye mesh screen sieves;
Ratio in solid-liquid mass ratio 1:25-35 adds Pericarpium Citri Reticulatae Viride powder and acetone in container, the concentration of acetone is 70-90%, and solution is at constant temperature 40-50 ℃ of following oscillation treatment 10-14h;
Above-mentioned solution centrifugal is handled 2-4 time, the assorted supernatant of collecting of filter;
Supernatant concentrating under reduced pressure under 55-65 ℃ of temperature obtains ointment;
Press 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. hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment is characterized in that may further comprise the steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
Pulverizing back 70-90 eye mesh screen sieves;
Ratio in solid-liquid mass ratio 1:25-35 adds Pericarpium Citri Reticulatae Viride powder and acetone in container, the concentration of acetone is 70-90%, and solution is at constant temperature 40-50 ℃ of following oscillation treatment 10-14h;
Above-mentioned solution centrifugal is handled 2-4 time, the assorted supernatant of collecting of filter;
In supernatant, repeatedly add the floccule that ethanol that concentration is 80-95% and filtering occur, till no floccule appearance;
Solution concentrating under reduced pressure under 55-65 ℃ of temperature that will add behind the ethanol obtains ointment;
Press 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. hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment is characterized in that may further comprise the steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
Pulverizing back 70-90 eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed container, in the ratio adding pure water of solid-liquid mass ratio 1:8-12;
Adding concentration in above-mentioned solution is that 1-2.5g/L is with any pectase and cellulase than mixing, ratio with the volume ratio 1:90-110 of enzyme and solution adds, the ph value of solution is transferred to behind the 5.5-6.7 with seal of vessel oscillation treatment 36-60h under 30-50 ℃ of constant temperature;
Adding concentration in the solution behind enzymolysis is the acetone of 70-90%, is that the ratio of 1:12-18 adds with the volume ratio of acetone and enzymolysis solution, and solution is at constant temperature 40-50 ℃ of following oscillation treatment 10-14h;
The solution centrifugal that adds behind the acetone is handled 2-4 time, the assorted collection of filter supernatant;
In supernatant, repeatedly add the floccule that ethanol that concentration is 80-95% and filtering occur, till no floccule appearance;
Solution concentrating under reduced pressure under 55-65 ℃ of temperature that will add behind the ethanol obtains ointment;
Press 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. hair dye preparation method based on the Exocarpium Juglandis Immaturus pigment is characterized in that may further comprise the steps:
Strip Exocarpium Juglandis Immaturus, dry in shady spot;
Pulverizing back 70-90 eye mesh screen sieves;
Exocarpium Juglandis Immaturus powder after sieving is placed container, in the ratio adding pure water of solid-liquid mass ratio 1:8-12;
Adding concentration in above-mentioned solution is that 1-2.5g/L is with any pectase and cellulase than mixing, ratio with the volume ratio 1:90-110 of enzyme and solution adds, the ph value of solution is transferred to behind the 5.5-6.7 with seal of vessel oscillation treatment 36-60h under 30-50 ℃ of constant temperature;
Solution behind the enzymolysis places on the microwave ultrasonic wave extraction apparatus, and microwave power is made as 100-250W, and ultrasonic frequency is made as 20-30KHz, and ultrasonic power is made as 900-1200W, and the time is 20-36min;
Adding concentration in the solution behind enzymolysis is the acetone of 70-90%, is that the ratio of 1:12-18 adds with the volume ratio of acetone and enzymolysis solution, and solution is at constant temperature 40-50 ℃ of following oscillation treatment 10-14h;
The solution centrifugal that adds behind the acetone is handled 2-4 time, the assorted collection of filter supernatant;
In supernatant, repeatedly add the floccule that alcohols material that concentration is 80-95% and filtering occur, add alcohols material till no floccule appearance;
Solution concentrating under reduced pressure under 55-65 ℃ of temperature that will add behind the ethanol obtains ointment;
Press 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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