CN113549502A - Formula and preparation method of liquid detergent containing gleditschia horrida saponin - Google Patents

Abstract

The invention belongs to the field of fine chemical engineering, and particularly relates to a formula and a preparation method of common liquid detergent and concentrated liquid detergent containing gleditschia horrida saponin. The gleditsia sinensis has good washing and protecting capacity, and is applied as a natural washing and protecting agent from the ancient times in China. The invention provides application of gleditschia horrida saponin in a liquid detergent, designs formulas and preparation methods of a common liquid detergent and a concentrated liquid detergent containing the gleditschia horrida saponin, and proves that the two types of liquid detergents have good use effects, meet market demands and have practical production and application potentials through various experiments.

Description

Formula and preparation method of liquid detergent containing gleditschia horrida saponin

Technical Field

The invention belongs to the field of fine chemical engineering, and particularly relates to a formula and a preparation method of a liquid detergent containing gleditschia horrida saponin.

Background

Gleditsia fruit (Chinese honey locust)Gleditsia sinensisLam.) is a plant belonging to the genus Gleditsia of the family Leguminosae, about 16 kinds of which are widely distributed all over the world, wherein Gleditsia sinensis is the most widely distributed, belongs to the special species of China, and covers most of the regions of southeast, southwest and northwest. The gleditsia sinensis trees mostly grow in plains, valleys and hilly areas, like light and slightly shade, like warm and humid climates, are cold and dry resistant, can grow on limestone mountains and calcareous soil, can grow into big trees on light saline-alkali soil, and have the service life of six to seven hundred years. The fruit of Chinese honeylocust tree, Gleditsia sinensis, is rich in saponin, phenols and amino acids, and also contains various components such as ceryl alcohol, n-heptacosane, nonacosane, sitosterol, stigmasterol and tannin, wherein the saponin content is most abundant, which not only has good decontamination capability and foamability, but also can sterilize, remove dandruff and promote skin blood circulation, and can be used for cleaning underwear, skin, hair and food tablewareThe detergent is a natural surface active component and can be widely applied to the fields of daily chemicals and washing products.

The term "Saponin" is translated from the name Saponin, also known as Saponin, etc., and is a glycoside compound whose aglycone is triterpene or spirostane, and is composed of Saponin element and saccharide. The sugar chain comprises one or more linear oligosaccharides with a chain length varying from 2 to 5 sugar units; the sapogenin element (27 carbon sterol or 30 carbon triterpene) contains a multiple ring system. Since ancient times, the cleaning and protecting effects of the saponin of the gleditschia horrida have been discovered, and the folpet horrida is a custom for washing hair and clothes by boiling water in the gleditschia horrida from ancient times in China. Nowadays, many natural raw materials meeting the consumption trend are gradually excavated and used, and the gleditsia sinensis is urgently developed and utilized as a natural washing and protecting plant raw material with remarkable efficacy. The traditional Chinese honey locust extract has the advantages of no purification and decoloration, complex components, darker color and poor stability, and indexes such as foamability, washing ability, use experience and the like of the traditional Chinese honey locust extract are not evaluated after the traditional Chinese honey locust extract is added into a formula for use. Through the improvement and optimization of the extraction process, the gleditsia sinensis saponin is light yellow powder, the purity is 98.6%, the stability is good, the water solubility is good, and no peculiar smell exists. In combination with the cost consideration, the gleditschia horrida saponin is compounded into daily chemical washing products, various indexes of the gleditschia horrida saponin are explored, and reference is provided for developing the daily chemical products containing the gleditschia horrida saponin.

In addition, with the higher requirement of the current society on environmental protection by the large environment, the environmental protection index is also an important point of purchase when consumers purchase washing products, however, the Ethylene Diamine Tetraacetic Acid (EDTA) is added to the washing and nursing products in the current market, although EDTA is an ideal complexing agent, can form a complex with most metals, is widely applied to the detergent production industry, but is difficult to biodegrade in the environment, and the EDTA must not be added to the tableware detergent, the personal hygiene detergent and the household detergent products which are clearly specified in the technical requirement for the authentication of the washing products in China.

Disclosure of Invention

The invention provides a safe and reliable formula of a liquid detergent and a preparation method thereof by fully combining the application history and the practical advantages of the gleditsia sinensis, aiming at the problem that the domestic market lacks systematic and effective gleditsia sinensis washing products at present. The liquid detergent prepared by the formula has the characteristics of strong detergency, mildness, no damage to hands, clarity, transparency and pleasant smell, can effectively clean various stains including oil stains, blood stains and fruit and vegetable juice, and has good feedback for testees. In addition, in view of the possible environmental risk of EDTA, the formula adopts biodegradable chelating agent tetrasodium glutamate diacetate instead of (GLDA, N, N-BIS (CARBOXYMETHYL) -L-GLUTAMIC) EDTA-2Na, and provides safer and more reassuring quality for users on the basis of ensuring the original complexing efficacy.

In order to achieve the purpose, the invention provides the following technical scheme:

1. the formula of the ordinary liquid detergent (active matter is more than or equal to 15%) containing the gleditschia horrida saponin is as follows:

0.1-0.3% of tetrasodium glutamate diacetate, 12.0-16.0% of sodium lauryl alcohol ether sulfate, 92.0-4.0% of fatty alcohol-polyoxyethylene ether, 2.0-5.0% of coconut oil fatty acid diethylamide, 0.2-0.7% of hydrophobically modified acrylic polymer, 0.4-0.9% of potassium hydroxide, 0.5-1.5% of gleditsia sinensis saponin, 0.05-0.2% of kathon, 0.2-0.5% of essence and 2.0-3.0% of sodium chloride. The optimal formula of the common gleditschia horrida saponin detergent comprises the following components: 0.2% of tetrasodium glutamate diacetate, 15.0% of sodium dodecyl alcohol ether sulfate, 93.0% of fatty alcohol-polyoxyethylene ether, 3.0% of coconut oil fatty acid diethylamide, 0.5% of hydrophobically modified acrylic polymer, 0.6% of potassium hydroxide, 1% of gleditsia sinensis saponin, 0.1% of kasong, 0.3% of essence and 2.2% of sodium chloride.

2. The formula of the concentrated liquid detergent containing the gleditschia horrida saponin (the active matter is more than or equal to 25 percent) is as follows: 1.0-2.0% of tetrasodium glutamate diacetate, 20.0-30.0% of polyethoxylated fatty alcohol, 3.0-8.0% of branched-chain fatty alcohol alkoxy, 3.0-6.0% of glycerol, 0.5-0.8% of acrylic acid homopolymer, 0.1-0.3% of cason, 0.3-1.2% of compound protease, 0.5-1.5% of gleditsia sinensis saponin and 0.2-0.6% of kumquat essence. The optimal formula of the concentrated type liquid detergent containing the gleditschia horrida saponin comprises the following components: 1.2% of tetrasodium glutamate diacetate, 25.0% of polyethoxylated fatty alcohol, 5.0% of branched-chain fatty alcohol alkoxy, 5.0% of glycerol, 1.0% of acrylic acid homopolymer, 0.1% of cason, 1% of compound protease, 1% of gleditsia sinensis saponin and 0.3% of kumquat essence.

3. The preparation method of the common liquid detergent containing the gleditschia horrida saponin comprises the following steps:

1) sequentially adding tetrasodium glutamate diacetate, sodium lauryl ether sulfate, fatty alcohol-polyoxyethylene ether-9 and coconut oil fatty acid diethylamide at 80 ℃, and stirring until the tetrasodium glutamate diacetate, the sodium lauryl ether sulfate, the fatty alcohol-polyoxyethylene ether-9 and the coconut oil fatty acid diethylamide are completely dissolved;

2) cooling to 45 ℃, adding the hydrophobic modified acrylic polymer which is pre-diluted, and uniformly stirring;

3) adding potassium hydroxide, and adjusting the pH value to about 7.5;

4) adding Gleditsia Saponin, Kathon, essence and sodium chloride, and stirring;

5) measuring pH and viscosity, and aseptic canning.

4. The preparation method of the concentrated liquid detergent containing the gleditschia horrida saponin comprises the following steps:

1) mixing polyethoxylated fatty alcohol with branched fatty alcohol alkoxy, and stirring uniformly;

2) slowly adding water, and uniformly stirring again;

3) sequentially adding tetrasodium glutamate diacetate and glycerol, and uniformly stirring;

4) adding acrylic acid homopolymer and stirring uniformly;

5) sequentially adding the kalong, the compound protease, the gleditsia sinensis saponin and the kumquat essence, and uniformly stirring;

6) tetrasodium glutamate diacetate was added to adjust the pH to about 7.5.

Drawings

FIG. 1 results of foam height measurement of general type liquid detergent containing saponin of Gleditsia sinensis

FIG. 2 height measurement of concentrated liquid soap foam from Gleditsia sinensis Saponin

FIG. 3 shows the result of the detergency of concentrated type liquid detergent containing saponin of Gleditsia sinensis

FIG. 4 results of the detergency test of general type liquid detergent containing saponin of Gleditsia sinensis

FIG. 5 shows the radar chart of the human body test evaluation of the general type liquid detergent of gleditschia horrida saponin

FIG. 6 shows radar chart for human trial evaluation of concentrated Gleditsia sinensis saponin type liquid detergent

Detailed description of the preferred embodiments

EXAMPLES example 1 shampoo Performance testing

1.1 protocol

Height of foam

The common type and the concentrated type liquid detergent samples are respectively and uniformly mixed with water (1: 4) to obtain 20 percent liquid to be detected. And (3) sucking 1mL of solution to be detected (20%) and adding the solution to the test tube with the scale, uniformly shaking for 30 times by a hand shaking method, recording the foam height, measuring the foam height for three times, taking the average value and recording the average value as H, and comparing with a liquid detergent without the saponin of the gleditschia horrida (except the saponin of the gleditschia horrida, the other components are the same).

Soil-release capacity test

According to the following steps of 1: a washing solution of 300 mL was prepared by mixing a normal type and a concentrated type of detergent with water at a ratio of 100. Respectively spraying artificial stains on clean plastic bowls, metal bowls, wooden bowls and porcelain bowls (respectively weighing m), and naturally drying in the air (weighing m)₁) Then washing, soaking in washing liquid for 1min, rinsing for 3 min at 30 deg.C, quickly taking out the washed bowl, hanging in the air for 3 hr, and weighing to obtain a weight m₂. The loss of oil stain weight was evaluated for the stain removal of two detergents, and averaged in 3 parallel runs with the control being a detergent without the addition of saponin (except for saponin, the other ingredients were the same). The formula for calculating detergency is as follows:

(artificial dirt: weighing 8.0 g of vegetable oil, 1.5 g of carbon powder, 0.05 g of liquid paraffin and 1mL of fruit juice, and stirring the mixture evenly by using a glass rod before each use).

1.2 results of the experiment

The result shows that the foaming capacity and the decontamination capacity of the formula can be obviously improved by adding the gleditschia horrida saponin, the washing capacity of the traditional chemical cleaning and caring products is effectively improved, and the detergent prepared by the formula has good foaming capacity and decontamination capacity after the gleditschia horrida saponin is added.

Example 2 physicochemical indices

Sensory indexes of the gleditsia sinensis saponin ordinary type detergent and the sensory and physical and chemical properties of the gleditsia sinensis saponin concentrated type detergent are recorded through observation and trial, and are comprehensively evaluated according to GB9985-2000 and GB/T13173.2-91 standards. And performing stability test, respectively placing the two kinds of liquid detergents at high temperature (40 +/-2 ℃) and low temperature (-5 +/-2 ℃) for three months, and observing whether the two kinds of liquid detergents have layering and discoloration phenomena.

Example 3 microorganism and heavy Metal indicators

Referring to the specification of GB9985-2000 on the detergent, the microbial content and the heavy metal content of the two detergents are measured.

Example 4 safety test

4.1 Experimental methods

4.1.1 Trypan blue staining method (CAM-TBS)

1) Selecting SPF eggs to hatch, observing the eggs after 10 days of incubation by light source irradiation, wherein the hatching conditions are as follows: the temperature is 37-38 ℃, and the relative humidity is 60%;

2) selecting eggs which are normally developed, and peeling off eggshells at the positions of air chambers, wherein every three eggs form a group;

3) dropping physiological saline on the egg membrane, peeling off the egg membrane to expose the allantoic membrane (CAM), and placing a plastic ring with diameter of 1.5cm thereon;

4) dripping 200 μ L of sample into the ring, and taking the other two eggs as positive control and negative control respectively, wherein physiological saline is dripped into the positive control, 1% SDS is dripped into the positive control, and the eggs are washed after being exposed for 20s respectively;

5) continuously dripping 500 mu L of 0.1% trypan blue dye solution into the circle, exposing for 1min, and washing for 20s with physiological saline;

6) shearing an exposed area, placing the area into 5 mL of formamide, standing overnight, centrifuging at 3000 r/min for 5 min, removing supernatant, placing the supernatant into an enzyme-linked immunosorbent assay, and measuring the absorbance at 595 nm;

7) respectively making into concentration of 1 × 10^-6，5×10^-6，1×10^-5And 5X 10^-5And (3) a standard curve of trypan blue dye in mol/L and corresponding absorbance. The standard curve equation is: y =36.6375x +0.0922, R²=0.9993；

8) Recording data, calculating the concentration value (A value, mol/L) of trypan blue dye in the supernatant through a standard curve, and the quantity (D value, nmol) of trypan blue absorbed after the CAM is injured by stimulation

。

Skin patch experiment

1) Selecting at least 30 persons with physical health meeting the test condition, and at least 30 persons;

2) the selected area is not more than 50mm²Qualified spot test equipment with the depth of about 1 mm;

3) putting the test object into a small chamber of a spot tester, wherein the dosage is about 0.020 mL-0.025 mL, and no substance is added into a control hole;

4) applying the spot test device with the test object on the back or forearm curve side of the test object with hypoallergenic adhesive tape, and lightly pressing with palm to uniformly apply on the skin for 24 h;

5) the skin reactions were observed according to the standard of table 6 30 min (after disappearance of the indentation), 24 h and 48 h after removal of the test article plaque test device, respectively, and the observation results were recorded.

4.2 results of the experiment

The result shows that the stimulating grading result of the liquid detergent added with the saponin of the gleditschia horrida is no/slight stimulation in the trypan blue staining experiment, and no adverse reaction occurs in the skin closed patch experiment within 0-48 h.

Example 5 human trial evaluation

The two kinds of liquid detergents aim at fully cleaning oil stains on bowls and chopsticks, are mild and do not hurt hands, and the specific indexes comprise: the detergent power, the mildness, the foam abundance, the easy bleaching property, the odor removing effect and the smell are seven items.

Randomly selecting 40 people, half men and women, and continuously using the self-made liquid detergent containing the gleditschia horrida saponin for five times with the age of 20-40 years, washing according to the same method, adding used metal bowls/wooden bowls/plastic bowls and porcelain bowl seeds for washing each time, and finally performing sensory comparison and scoring according to the hair washing effect of the product. And taking 10 points, 1 point is worst, 10 points is best, and the average value of the comprehensive data. The result shows that the seven indexes have good overall performance, are consistent and certain to volunteers, and have potential of being put into practical production and development.

Claims (10)

1. The liquid detergent containing the saponin of the gleditschia horrida is characterized by containing the saponin of the gleditschia horrida as a natural surfactant, so that the washing capacity of the liquid detergent is enhanced, and the product has good use experience.

2. The detergent according to claim 1, wherein the gleditschia horrida saponin accounts for 1% of the total mass of the detergent.

3. Use of Gleditsia Saponin in preparing washing product is provided.

4. Use of saponin from Gleditsia sinensis in preparing product with washing ability is provided.

5. The formula of the ordinary liquid detergent (active matter is more than or equal to 15%) containing the gleditschia horrida saponin is as follows: 0.1-0.3% of tetrasodium glutamate diacetate, 12.0-16.0% of sodium lauryl alcohol ether sulfate, 92.0-4.0% of fatty alcohol-polyoxyethylene ether, 2.0-5.0% of coconut oil fatty acid diethylamide, 0.2-0.7% of hydrophobically modified acrylic polymer, 0.4-0.9% of potassium hydroxide, 0.5-1.5% of gleditsia sinensis saponin, 0.05-0.2% of kathon, 0.2-0.5% of essence and 2.0-3.0% of sodium chloride.

6. The optimal formula of the common gleditschia horrida saponin detergent comprises the following components: 0.2% of tetrasodium glutamate diacetate, 15.0% of sodium dodecyl alcohol ether sulfate, 93.0% of fatty alcohol-polyoxyethylene ether, 3.0% of coconut oil fatty acid diethylamide, 0.5% of hydrophobically modified acrylic polymer, 0.6% of potassium hydroxide, 1% of gleditsia sinensis saponin, 0.1% of kasong, 0.3% of essence and 2.2% of sodium chloride.

7. The formula of the concentrated liquid detergent containing the gleditschia horrida saponin (the active matter is more than or equal to 25 percent) is as follows: 1.0-2.0% of tetrasodium glutamate diacetate, 20.0-30.0% of polyethoxylated fatty alcohol, 3.0-8.0% of branched-chain fatty alcohol alkoxy, 3.0-6.0% of glycerol, 0.5-0.8% of acrylic acid homopolymer, 0.1-0.3% of cason, 0.3-1.2% of compound protease, 0.5-1.5% of gleditsia sinensis saponin and 0.2-0.6% of kumquat essence.

8. The optimal formula of the concentrated type liquid detergent containing the gleditschia horrida saponin comprises the following components: 1.2% of tetrasodium glutamate diacetate, 25.0% of polyethoxylated fatty alcohol, 5.0% of branched-chain fatty alcohol alkoxy, 5.0% of glycerol, 1.0% of acrylic acid homopolymer, 0.1% of cason, 1% of compound protease, 1% of gleditsia sinensis saponin and 0.3% of kumquat essence.

9. The preparation method of the common liquid detergent containing the gleditschia horrida saponin comprises the following steps:

1) sequentially adding tetrasodium glutamate diacetate, sodium lauryl ether sulfate, fatty alcohol-polyoxyethylene ether-9 and coconut oil fatty acid diethylamide at 80 ℃, and stirring until the tetrasodium glutamate diacetate, the sodium lauryl ether sulfate, the fatty alcohol-polyoxyethylene ether-9 and the coconut oil fatty acid diethylamide are completely dissolved;

2) cooling to 45 ℃, adding the hydrophobic modified acrylic polymer which is pre-diluted, and uniformly stirring;

3) adding potassium hydroxide, and adjusting the pH value to about 7.5;

4) adding Gleditsia Saponin, Kathon, essence and sodium chloride, and stirring;

5) measuring pH and viscosity, and aseptic canning.

10. The preparation method of the concentrated liquid detergent containing the gleditschia horrida saponin comprises the following steps:

1) mixing polyethoxylated fatty alcohol with branched fatty alcohol alkoxy, and stirring uniformly;

2) slowly adding water, and uniformly stirring again;

3) sequentially adding tetrasodium glutamate diacetate and glycerol, and uniformly stirring;

4) adding acrylic acid homopolymer and stirring uniformly;

5) sequentially adding the kalong, the compound protease, the gleditsia sinensis saponin and the kumquat essence, and uniformly stirring;

6) tetrasodium glutamate diacetate was added to adjust the pH to about 7.5.

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