CN111171953A - Optimization method of cosmetic-grade camellia oil decoloring process - Google Patents

Optimization method of cosmetic-grade camellia oil decoloring process Download PDF

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CN111171953A
CN111171953A CN202010030121.6A CN202010030121A CN111171953A CN 111171953 A CN111171953 A CN 111171953A CN 202010030121 A CN202010030121 A CN 202010030121A CN 111171953 A CN111171953 A CN 111171953A
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decoloring
oil
decolorization
camellia oil
cosmetic
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杨选
王晔洋
黄莎
李伟荣
刘觉天
陈国宝
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Lishui Academy Of Agricultural And Forestry Sciences
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Lishui Academy Of Agricultural And Forestry Sciences
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/10Refining fats or fatty oils by adsorption

Abstract

The invention discloses a cosmetic-grade camellia oil decoloring process optimization method, and belongs to the technical field of camellia oil decoloring. The camellia oil decoloring process is optimized by the steps of deacidifying and washing crude oil → activating decolorant → decoloring rate measurement → single factor test → orthogonal test → data processing and the like. The decoloring process can effectively improve the decoloring rate of the camellia oil, ensure that the color of the camellia oil basically reaches colorless transparency, meets the requirement of cosmetic grade, and can effectively remove harmful components such as benzopyrene and the like in the camellia oil. In addition, the invention has moderate process temperature and simple operation.

Description

Optimization method of cosmetic-grade camellia oil decoloring process
Technical Field
The invention belongs to the technical field of camellia oil decoloration, and particularly relates to a cosmetic-grade camellia oil decoloration process optimization method.
Background
The oil and fat consists of triglyceride, and the pure triglyceride is colorless and transparent in liquid state and white in solid state. The process of removing pigment to improve the color of the grease is decolorization. Although the color of the oil is improved in the degumming and deacidification processes, the color is deep, and the chlorophyll pigments remained in the oil seeds are difficult to remove by methods except the adsorption method. The camellia oil has the characteristics of strong permeability, high oxidative stability, safety, no toxic or side effect and the like, is easy to be absorbed by skin, and has wide application in cosmetics and medicines. The color is an important index of cosmetic oil, and common cosmetic camellia oil is required to be colorless and transparent in sense. The camellia oil needs to achieve an ideal decoloring effect, and the key technology is to select a proper decoloring agent and process operation conditions. The adsorption decoloring can remove pigment, and can remove residual trace soapstock, colloid such as phospholipid and the like, polycyclic aromatic hydrocarbon and the like in the camellia oil.
The invention adopts an adsorption method to remove pigments in the camellia oil, so that the color of the camellia oil is nearly colorless, the requirement of cosmetic oil is met, and a certain theoretical basis is provided for industrialization of the camellia oil.
Disclosure of Invention
The invention aims to solve the defects of the prior art, provides an optimization method of a cosmetic-grade camellia oil decoloring process, and provides a certain theoretical basis for industrialization of camellia oil.
The invention adopts the following technical scheme:
the optimization method of the cosmetic-grade camellia oil decoloring process comprises the following steps:
step one, deacidifying and washing crude oil;
step two, activating a decolorizing agent;
step three, a decoloring process: placing deacidified oil and a certain amount of decolorizing agent in a suction filtration container, heating to a certain temperature, vacuumizing, decolorizing under vacuum state, and stirring; after a certain time, the decolorizing process is completed, and the decolorized oil is obtained by filtering;
step four, determining the decolorization rate: measuring the decolorization rate by adopting a spectrophotometry method, respectively measuring the light absorption values of the decolorized camellia oil and the crude oil at the maximum absorption wavelength after the crude oil is scanned at the full wavelength, and calculating the decolorization rate;
step five, single factor test: respectively researching the influence of different decolorants, the proportion of a composite decolorant, the decoloring temperature, the decoloring time, the consumption of the decolorant and the decoloring stirring speed on the decoloring effect, determining the factors influencing the decoloring effect, and then carrying out orthogonal test optimization;
step six, orthogonal test: on the basis of the single-factor test, the optimum adding amount of a decoloring agent, the decoloring time, the decoloring temperature and the decoloring stirring speed are used as intermediate values, the decoloring rate is used as an index, and L is designed9(34) Performing orthogonal test to determine the optimal decoloring production process;
step seven, data processing: each set of experiments was repeated three times, data was analyzed for variance, and results were analyzed statistically.
Further, the deacidifying of the crude oil in the first step is specifically as follows: firstly, measuring the acid value of crude oil, and calculating the alkali adding amount; stirring and heating the crude oil to 35-45 ℃, adding water according to the calculated alkali adding amount to prepare 10% alkali liquor, uniformly spraying the alkali liquor into the oil, fully stirring and mixing, heating to 50-60 ℃, reducing the stirring speed when nigre floccule coagulates appear in the oil, promoting the floccules to further coagulate, stopping stirring, and standing at constant temperature for 8-12 hours;
the step one of water washing specifically comprises the following steps: transferring the upper layer clear oil into a container, heating the oil to 75-85 ℃, simultaneously adding 75-85 ℃ distilled water accounting for 10% of the mass of the clear oil for washing, stirring for 10-20min at a speed of 100r/min, standing, separating out waste water, dropwise adding phenolphthalein, discarding the waste water, carrying out secondary washing, stopping washing when the phenolphthalein does not change color in the waste water, and dehydrating and drying the washed clear oil under a vacuum condition to obtain deacidified washed oil for decolorization.
Further, the activation decolorant in the second step is specifically: drying activated carbon and activated clay in a drying oven at 105 ℃ for 1-2h, cooling, and placing in a dryer.
Further, in the fifth step, the decolorant is activated clay, attapulgite or activated carbon.
Further, in the fifth step, the compound decolorant is clay: activated carbon, clay: the mass ratio of the activated carbon is 20:1, 10:1 and 5: 1. 4:1, 3:1, 2:1, 1: 1; in the fifth step, the decoloring temperature is 60 ℃, 70, 80, 90 and 100 ℃ respectively; in the fifth step, the decoloring time is respectively 5min, 10 min, 15min, 20min and 25 min; in the fifth step, the addition amounts of the decoloring agents are respectively 1%, 2%, 3%, 4%, 5% and 6%; and in the fifth step, the decoloring stirring speed is respectively 50, 100, 150, 200 and 250 r/min.
Further, in the sixth step, four-factor three-level orthogonal tests are carried out by selecting the decoloring temperature (80 ℃, 90 ℃ and 100 ℃), the decoloring time (15, 20 and 25min), the adding amount of the decoloring agent (4%, 5% and 6%) and the stirring speed (50r/min, 100r/min and 150 r/min).
Furthermore, the optimal decoloring production process in the sixth step is that the decoloring temperature is 90 ℃, the decoloring time is 20min, the addition amount of the decoloring agent is 6%, and the stirring speed in the decoloring process is 150 r/min.
Compared with the prior art, the invention has the beneficial effects that: the decoloring process can effectively improve the decoloring rate of the camellia oil, ensure that the color of the camellia oil basically reaches colorless transparency, meets the requirement of cosmetic grade, and can effectively remove harmful components such as benzopyrene and the like in the camellia oil. In addition, the invention has moderate process temperature and simple operation.
Drawings
FIG. 1 is a visible light spectral scan;
FIG. 2 is a graph showing the effect of different decolorizing agents on decolorization rate;
FIG. 3 shows the effect of different ratios of compound decolorants on the decolorization ratio;
FIG. 4 effect of different decolorizing temperatures on decolorizing ratio;
FIG. 5 is a graph showing the effect of different bleaching times on the bleaching rate;
FIG. 6 shows the effect of different amounts of decolorizing agents on decolorization;
FIG. 7 shows the effect of different stirring speeds on decolorization ratio.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, which is defined in the appended claims, as may be amended by those skilled in the art upon reading the present invention.
1 materials and methods
1.1 test materials
Crude oil: camellia oil, ltd, zhejiang; activated carbon: liyang city rising activated carbon plant; activated clay: obobard adsorption materials, Inc., Wuxi; attapulgite clay: obobard adsorption materials, Inc., Wuxi; sodium hydroxide: chemical agents of the national drug group, ltd.
1.2 instrumentation
TU-1810PC UV-Vis Spectrophotometer: beijing general analysis general instruments, Inc.; circulating water vacuum pump: shanghaineqi science and technology, Inc.; ZNCL-heat collection type magnetic stirrer: consumer Provisions of Waals Instrument Limited.
1.3 test methods
1.3.1 crude oil deacidification process
Firstly, measuring the acid value of crude oil, and calculating the alkali adding amount according to the following formula: base addition 0.713 acid value crude oil quality 10-3+ crude oil mass 0.1%. Heating crude oil to 35 deg.C in magnetic stirrer, adding 10% alkali solution prepared by calculated alkali addition amount, adding water, uniformly spraying into oil, stirring, mixing, heating to 55 deg.C, reducing stirring speed when flocculent coagulate of soapstock appears in oil, stopping stirring, and standing at constant temperature for 10 hr (depending on whether soapstock is completely precipitated).
Washing with water: transferring the upper layer clear oil to a washing pot, heating the oil to 80 ℃, simultaneously adding 10% of 80 ℃ distilled water for washing, stirring for 10-20min at a speed of 100r/min, standing by using a separating funnel, separating the wastewater, dropwise adding phenolphthalein, discarding the wastewater, performing secondary washing, and stopping washing when the phenolphthalein does not change color in the wastewater. And (3) dehydrating and drying the washed clear oil under a vacuum condition to obtain the deacidified washed oil for decolorization.
1.3.2 activation of decolorizing agent: respectively taking a certain amount of active carbon and active clay, drying in a drying oven at 105 ℃ for 2h, cooling, and then placing in a dryer.
1.3.3 decolorization Process
Putting 50g of deacidified oil and a certain amount of decolorant in a filter flask, heating to a certain temperature, vacuumizing, decoloring in a vacuum state, and stirring; and (4) finishing the decoloring process after a certain time, and filtering to obtain decolored oil.
1.3.4 determination of decolorization ratio
The decolorization rate is determined by spectrophotometry. And after the crude oil is scanned at full wavelength, respectively measuring the light absorption values of the decolorized camellia oil and the crude oil at the maximum absorption wavelength, and calculating the decolorization rate. The decolorization ratio calculation formula is:
decolorization ratio/% (A1-A2)/A1X 100%
Wherein: a1 is the absorbance of crude oil; a2 is the absorbance of decolorized camellia oil.
1.3.5 Single factor test
The influence of different decolorants, the proportion of a composite decolorant, the decoloring temperature, the decoloring time, the consumption of the decolorant and the decoloring stirring speed on the decoloring effect is respectively researched, the factors influencing the decoloring effect are determined, and then orthogonal test optimization is carried out.
1.3.6 orthogonal test
On the basis of single factor, the optimum adding amount of a decolorizing agent, decolorizing time, decolorizing temperature and decolorizing stirring speed are used as intermediate values, the decolorizing rate is used as an index, and L is designed9(34) And performing orthogonal test to determine the optimal decoloring production process. The experimental design is shown in table 1.
Table 1 design of orthogonal experiments
Figure BDA0002363141120000041
1.3.7 data processing
Each group of experiments was repeated 3 times, and data was analyzed for variance using a sps and results were analyzed statistically using Excel.
2 results and analysis
2.1 determination of the maximum absorption wavelength
The wavelength of crude oil is scanned within the range of 400-700 nm by using distilled water as a reference, and the maximum absorption wavelength is determined, and the result is shown in figure 1. As can be seen from FIG. 1, the maximum absorption wavelength of camellia oil is 455 nm. The maximum absorption wavelength may be different due to different oil products, and the result is different from other documents, the maximum wavelength measured by Wujianbao et al is 430nm, and the maximum wavelength measured by the Sun Shi Fang is 480 nm.
2.2 analysis of Single-factor test results
2.2.1 Effect of different decolorizing agents on decolorization Rate
Three decolorants, namely activated clay, attapulgite and activated carbon, were selected for carrying out a decoloration test under the conditions of decolorant dosage of 2%, decoloration temperature of 80 ℃, decoloration time min and stirring speed of 100r/min, and the results are shown in fig. 2. As can be seen from FIG. 2, the decolorization ratio of the three decolorizers is 93%, and the decolorization effect has no significant difference. Therefore, activated clay is selected as the bleaching agent in view of the cost of practical production. And secondly, taking harmful substances such as benzopyrene which cannot be removed by the clay into consideration in the production process by using the activated carbon, so that the clay and the activated carbon are required to be compounded for use.
2.2.2 Effect of Compound decolorizer ratio on decolorization Rate
Selecting argil under the conditions that the addition amount of a compound decolorizing agent is 2 percent, the decolorizing temperature is 80 ℃, the decolorizing time is 15min and the stirring speed is 100 r/min: the ratio of the activated carbon is 20:1, 10:1 and 5: 1. the results of the decolorization tests were shown in FIG. 3 for 4:1, 3:1, 2:1, and 1: 1. As can be seen from FIG. 3, there is no significant difference between the decoloring effects of the compound decoloring agents in different proportions, so from the viewpoint of production economy, clay is selected: the ratio of activated carbon was 20: 1.
2.2.3 Effect of Decoloration temperature on Camellia oil Decoloration
Under the conditions that the ratio of the activated clay to the activated carbon is 20:1, the addition amount of a decolorizing agent is 2%, the stirring speed is 100r/min, and the decolorizing time is 15min, different decolorizing temperatures of 60, 70, 80, 90 and 100 ℃ are selected for carrying out a decolorizing test, and the result is shown in figure 4. As can be seen from fig. 4, the decoloring rate shows a trend of increasing significantly with the increase of the decoloring temperature, and when the temperature reaches 90 ℃, the decoloring rate reaches 94.66%, and then the decoloring rate does not change significantly. The decolorizer can be accelerated to contact with the colored substances of the oil by increasing the decolorization temperature, and the decolorization of the oil is accelerated. Too high temperature can also accelerate the oxidation of the tea oil and influence the quality of the tea oil. Thus temperatures generally do not exceed 100 ℃ in practice. Therefore 90 ℃ was chosen for subsequent orthogonal experiments.
2.2.4 Effect of Decoloration time on Decoloration
The decolorization test is carried out by selecting different decolorization temperatures of 5, 10, 15, 20 and 25min under the conditions that the ratio of activated clay to activated carbon is 20:1, the addition amount of a decolorizer is 2%, the decolorization temperature is 80 ℃ and the stirring speed is 100r/min, and the result is shown in figure 5. As can be seen from FIG. 5, the decolorization rate tended to increase significantly with the increase in the decolorization time, and the decolorization rate reached 95.03% at the decolorization time of 20min, and there was no significant difference thereafter. In the actual production process, the longer the time is, the tea oil can be slowly oxidized, and the production time generally does not exceed 30min, so the decolorization time is selected to be 20min for carrying out the subsequent orthogonal test.
2.2.5 Effect of decolorizing agent addition on decolorizing ratio
The decolorization test is carried out by selecting different addition amounts of 1%, 2%, 3%, 4%, 5% and 6% under the conditions of the ratio of the clay to the active carbon being 20:1, the decolorization temperature being 80 ℃, the stirring speed being 100r/min and the time being 15min, and the result is shown in figure 6. As can be seen from FIG. 6, the amount of the decoloring agent added significantly affects the decoloring effect. When the addition amount of the decoloring agent is in a range of 1-5%, the decoloring rate is increased along with the increase of the addition amount, when the addition amount of the decoloring agent is 1%, the decoloring rate is only 80.72%, when the use amount of the decoloring rate reaches 5%, the decoloring rate reaches 95.82%, and when the addition amount of the decoloring agent is 6% and 5%, no significant difference exists, so that an orthogonal test is carried out by selecting 5% of the use amount of the additive.
2.2.6 influence of stirring speed on decolorization rate of refined camellia oil in decolorization process
Under the conditions of the ratio of activated clay to activated carbon being 20:1, the addition of a decolorizing agent being 2%, the decolorizing temperature being 80 ℃ and the decolorizing time being 15min, different stirring speeds of 50, 100, 150, 200 and 250r/min are selected for carrying out decolorization tests, and the results are shown in figure 7. As can be seen from FIG. 7, the decoloring rate tends to increase and decrease with the increase of the decoloring time, and the decoloring rate reaches a maximum of 93.69% at a decoloring stirring speed of 100r/min, and decreases as the stirring speed continues to increase. The proper stirring can ensure that the decolorizing agent is fully contacted with the tea oil, and the decolorizing efficiency is improved. However, the stirring speed cannot be too high because the oxidation of the tea oil is accelerated by vigorous stirring, so that the decoloring stirring speed of 100r/min is selected for the subsequent orthogonal test.
2.3 analysis of orthogonal test results
According to the results of the single-factor test, the four-factor three-level orthogonal test analysis is carried out on the test by selecting the decoloring temperature (80, 90 and 100 ℃), the decoloring time (15, 20 and 25min), the decoloring agent adding amount (4, 5 and 6 percent) and the stirring speed (50, 100 and 150 r/min).
The results of the orthogonal experiments are shown in table 2. As can be seen from Table 2, the visual optimum combination is A2B2C3D1The decolorization ratio is 98.46 percent, and the range of the factors is RA>RC>RB>RDNamely, the factor A (decolorizing temperature) has the largest influence on the decolorizing effect of the camellia oil, and the factor C (decolorizing agent adding amount), the factor B (decolorizing time) and the factor D (stirring speed) have the smallest influence. The optimum combination of decolorizing conditions was obtained from the test results as A3B3C3D1Inconsistent with visual combination, after performing a verification test, A3B3C3D1The result of the verification test of (1) is 98.22%, and has no significant difference with the result of the direct optimal combination. From an economic point of view A2B2C3D1The combination is more reasonable. The optimum decolorization conditions for tea oil are therefore: the decoloring temperature is 90 ℃, the decoloring time is 20min, the addition amount of a decoloring agent is 6 percent, and the stirring speed in the decoloring process is 150 r/min.
TABLE 2 results of orthogonal experiments
Figure BDA0002363141120000061
The embodiments of the present invention have been described in detail with reference to the above examples, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.

Claims (7)

1. The optimization method of the cosmetic-grade camellia oil decoloring process is characterized by comprising the following steps:
step one, deacidifying and washing crude oil;
step two, activating a decolorizing agent;
step three, a decoloring process: placing deacidified oil and a certain amount of decolorizing agent in a suction filtration container, heating to a certain temperature, and adding water
Vacuumizing, decoloring in a vacuum state, and stirring; after a certain time, the decolorizing process is completed, and the decolorized oil is obtained by filtering;
step four, determining the decolorization rate: measuring the decolorization rate by adopting a spectrophotometry method, respectively measuring the light absorption values of the decolorized camellia oil and the crude oil at the maximum absorption wavelength after the crude oil is scanned at the full wavelength, and calculating the decolorization rate;
step five, single factor test: respectively researching the influence of different decolorants, the proportion of a composite decolorant, the decoloring temperature, the decoloring time, the consumption of the decolorant and the decoloring stirring speed on the decoloring effect, determining the factors influencing the decoloring effect, and then carrying out orthogonal test optimization;
step six, orthogonal test: on the basis of the single-factor test, the optimum adding amount of a decoloring agent, the decoloring time, the decoloring temperature and the decoloring stirring speed are used as intermediate values, the decoloring rate is used as an index, and L is designed9(34) Performing orthogonal test to determine the optimal decoloring production process;
step seven, data processing: each set of experiments was repeated three times, data was analyzed for variance, and results were analyzed statistically.
2. The method for optimizing the decoloring process of cosmetic-grade camellia oil according to claim 1, wherein the deacidification of the crude oil in the first step is specifically as follows: firstly, measuring the acid value of crude oil, and calculating the alkali adding amount; stirring and heating the crude oil to 35-45 ℃, adding water according to the calculated alkali adding amount to prepare 10% alkali liquor, uniformly spraying the alkali liquor into the oil, fully stirring and mixing, heating to 50-60 ℃, reducing the stirring speed when nigre floccule coagulates appear in the oil, promoting the floccules to further coagulate, stopping stirring, and standing at constant temperature for 8-12 hours;
the step one of water washing specifically comprises the following steps: transferring the upper layer clear oil into a container, heating the oil to 75-85 ℃, simultaneously adding 75-85 ℃ distilled water accounting for 10% of the mass of the clear oil for washing, stirring for 10-20min at a speed of 100r/min, standing, separating out waste water, dropwise adding phenolphthalein, discarding the waste water, carrying out secondary washing, stopping washing when the phenolphthalein does not change color in the waste water, and dehydrating and drying the washed clear oil under a vacuum condition to obtain deacidified washed oil for decolorization.
3. The method for optimizing the decoloring process of cosmetic-grade camellia oil according to claim 1, wherein the activation decoloring agent in the second step is specifically: drying activated carbon and activated clay in a drying oven at 105 ℃ for 1-2h, cooling, and placing in a dryer.
4. The optimization method for the decolorization process of cosmetic-grade camellia oil according to claim 1, wherein in the fifth step, the decolorizer is activated clay, attapulgite or activated carbon.
5. The optimization method for the decolorization process of cosmetic-grade camellia oil according to claim 1, wherein in the fifth step, the composite decolorizer is clay: activated carbon, clay: the mass ratio of the activated carbon is 20:1, 10:1 and 5: 1. 4:1, 3:1, 2:1, 1: 1; in the fifth step, the decoloring temperature is 60 ℃, 70, 80, 90 and 100 ℃ respectively; in the fifth step, the decoloring time is respectively 5min, 10 min, 15min, 20min and 25 min; in the fifth step, the addition amounts of the decoloring agents are respectively 1%, 2%, 3%, 4%, 5% and 6%; and in the fifth step, the decoloring stirring speed is respectively 50, 100, 150, 200 and 250 r/min.
6. The optimization method for the decolorization process of cosmetic-grade camellia oil according to claim 1, wherein in the sixth step, four-factor three-level orthogonal tests are performed by selecting the decolorization temperature (80 ℃, 90 ℃, 100 ℃), the decolorization time (15, 20, 25min), the addition amount of the decolorizer (4%, 5%, 6%), and the stirring speed (50r/min, 100r/min, 150 r/min).
7. The optimization method for the decolorization process of cosmetic-grade camellia oil according to claim 6, wherein the optimal decolorization production process in the sixth step is decolorization temperature of 90 ℃, decolorization time of 20min, 6% of decolorizing agent addition, and stirring speed in the decolorization process of 150 r/min.
CN202010030121.6A 2020-01-10 2020-01-10 Optimization method of cosmetic-grade camellia oil decoloring process Pending CN111171953A (en)

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Application publication date: 20200519