阅读说明：本技术 一种含有皂荚皂素的洗衣液配方及其配制方法 (Formula and preparation method of laundry detergent containing gleditschia horrida saponin ) 是由 陈殿松 束成杰 马世宏 李卓航 马玲 单承莺 聂韡 于 2021-08-18 设计创作，主要内容包括：本发明属于精细化工领域,具体来说是涉及含有皂荚皂素的普通型洗衣液和浓缩型洗衣液配方及配制方法。皂荚具有良好的洗护能力,我国自古就应用皂荚作为天然洗护剂,本发明将皂荚皂素与其他表面活性剂和调理剂等进行复配,在保证成本较低且对人体无副作用、对环境友好等优点的前提下,更可以充分发挥皂荚皂素洗涤优势,可以有效应对各类材质衣物,对各类常见污渍均有良好去污效果。本发明提供了皂荚皂素在洗衣液中的应用,并设计了含有皂荚皂素的普通型洗衣液和浓缩型洗衣液配方及配制方法,并通过多种实验证明两种洗衣液使用效果佳,符合市场需求,具有实际生产应用潜力。(The invention belongs to the field of fine chemical engineering, and particularly relates to a formula of a common laundry detergent and a concentrated laundry detergent containing saponin of gleditschia horrida and a preparation method thereof. The gleditschia horrida has good washing and protecting capacity, and since ancient times, the gleditschia horrida is used as a natural washing and protecting agent. The invention provides application of gleditschia horrida saponin in a laundry detergent, designs formulas and preparation methods of a common laundry detergent and a concentrated laundry detergent containing the gleditschia horrida saponin, and proves that the two laundry detergents have good use effects, meet market requirements and have practical production and application potentials through various experiments.)

1. The liquid laundry detergent containing the saponin of the gleditsia sinensis is characterized by containing the saponin of the gleditsia sinensis as a natural surfactant, enhancing the washing capacity of the liquid laundry detergent and enabling the product to have good use experience.

2. The laundry detergent of claim 1, wherein the saponin fraction of the Gleditsia sinensis is present in an amount of 1% by weight of the total laundry 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 a common laundry 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, 1.0-3.0% of cocamide DEA, 2.0-4.0% of cocamidopropyl betaine, 0.8-1.5% of acrylic acid homopolymer, 0.5-1.5% of QT-1821.5, 0.5-1.5% of gleditschia saponin, 0.02-0.08% of silicone oil defoamer, 0.05-0.2% of KASONG, 1.5-2.5% of sodium chloride, 0.2-0.5% of essence and 0.2-0.6% of sodium hydroxide.

6. The optimal formula of the common laundry detergent containing the gleditschia horrida saponin comprises the following components: 0.2% of tetrasodium glutamate diacetate, 14.0% of sodium dodecyl alcohol ether sulfate, 92.0% of fatty alcohol-polyoxyethylene ether, 2.0% of cocamide DEA, 2.0% of cocamidopropyl betaine, 1.0% of acrylic acid homopolymer, QT-1822.0%, 1% of gleditsia sinensis saponin, 0.05% of silicone oil defoamer, 0.1% of kasong, 2.0% of sodium chloride, 0.3% of essence and 0.4% of sodium hydroxide.

7. The formula of the concentrated laundry detergent containing the gleditschia horrida saponin (active matter is more than or equal to 25 percent) is as follows: 0.1-0.3% of tetrasodium glutamate diacetate, 15.0-20.0% of sodium lauryl alcohol ether sulfate, 96.0-8.0% of fatty alcohol-polyoxyethylene ether, 1.0-4.0% of biodegradable nonionic surfactant, 1.0-3.0% of branched fatty alcohol alkoxy, 2.0-4.0% of cocamidopropyl betaine, 0.8-1.5% of hydrophobically modified acrylic polymer, 0.5-1.5% of gleditsia sinensis saponin, 0.05-0.07% of silicone oil emulsion, 0.1-0.3% of kasong, 0.2-0.6% of essence, 0.3-0.6% of potassium hydroxide and 1-3% of sodium chloride.

8. The optimal formula of the concentrated laundry detergent containing the gleditschia horrida saponin comprises the following components: 0.2% of tetrasodium glutamate diacetate, 18.0% of sodium lauryl alcohol ether sulfate, 98.0% of fatty alcohol-polyoxyethylene ether, 2.0% of biodegradable nonionic surfactant, 4.0% of branched fatty alcohol alkoxy, 2.0% of cocamidopropyl betaine, 1.0% of hydrophobically modified acrylic polymer, 1.0% of gleditsia sinensis saponin, 0.05% of silicone oil emulsion, 0.1% of kasong, 0.3% of essence, 0.4% of potassium hydroxide and 2.2% of sodium chloride.

9. In the invention, the preparation method of the common type liquid soap detergent containing the gleditschia horrida saponin comprises the following steps: sequentially adding tetrasodium glutamate diacetate and sodium lauryl alcohol ether sulfate at 70-75 ℃, and stirring until the tetrasodium glutamate diacetate and the sodium lauryl alcohol ether sulfate are completely dissolved; cooling, sequentially adding fatty alcohol-polyoxyethylene ether-9, cocamide DEA and cocamidopropyl betaine, and uniformly stirring; cooling to 45 ℃, adding the pre-diluted acrylic acid homopolymer, and uniformly stirring; adding QT-182, gleditschia horrida saponin, a silicone oil defoaming agent, kasonong, sodium chloride and essence, and uniformly stirring; adding sodium hydroxide, and adjusting the pH value to about 7.5; measuring pH and viscosity, and aseptic canning.

10. The preparation method of the concentrated liquid laundry detergent containing the gleditschia horrida saponin comprises the following steps: completely dissolving tetrasodium glutamate diacetate, sodium dodecyl alcohol ether sulfate, fatty alcohol-polyoxyethylene ether-9, a biodegradable nonionic surfactant and branched fatty alcohol alkoxy at 70-75 ℃; cooling, sequentially adding the cocamidopropyl betaine and the hydrophobically modified acrylic polymer, and uniformly stirring; adding a proper amount of potassium hydroxide, and adjusting the pH value to 7.5; sequentially adding the gleditschia horrida saponin, the silicone oil emulsion, the kasong, the essence and the sodium chloride, and uniformly stirring; measuring pH and viscosity, and aseptic canning.

Technical Field

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

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, namely Chinese honeylocust, is rich in saponin, phenols and amino acids, and also contains various components such as ceryl alcohol, n-heptacosane, nonacosane, sitosterol, stigmasterol, tannin and the like, wherein the saponin content is most abundant, so that the Chinese honeylocust tree fruit not only has good decontamination capability and foamability, but also can sterilize and remove dandruff, promotes skin blood circulation, can be used for cleaning close-fitting clothes, skin, hair and food tableware, is a natural surface active component, can be widely applied to the field 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 laundry detergent formula 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 laundry detergent prepared by the formula has the characteristics of good detergency, easiness in rinsing, mildness, low irritation and pleasant fragrance, can be applied to clothes made of various materials, can effectively clean various stains including oil stains, blood stains and fruit and vegetable juice, and has generally good feedback of 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:

in the invention, the general formula of the gleditschia horrida saponin laundry detergent (active matter is more than or equal to 15%) 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, 1.0-3.0% of cocamide DEA, 2.0-4.0% of cocamidopropyl betaine, 0.8-1.5% of acrylic acid homopolymer, 0.5-1.5% of QT-1821.5, 0.5-1.5% of gleditschia saponin, 0.02-0.08% of silicone oil defoamer, 0.05-0.2% of KASONG, 1.5-2.5% of sodium chloride, 0.2-0.5% of essence and 0.2-0.6% of sodium hydroxide.

The optimal formula of the common gleditschia horrida saponin laundry detergent comprises the following components: 0.2% of tetrasodium glutamate diacetate, 14.0% of sodium dodecyl alcohol ether sulfate, 92.0% of fatty alcohol-polyoxyethylene ether, 2.0% of cocamide DEA, 2.0% of cocamidopropyl betaine, 1.0% of acrylic acid homopolymer, QT-1822.0%, 1% of gleditsia sinensis saponin, 0.05% of silicone oil defoamer, 0.1% of kasong, 2.0% of sodium chloride, 0.3% of essence and 0.4% of sodium hydroxide.

In the invention, the formula of the concentrated type liquid soap detergent containing the gleditschia horrida saponin (the active matter is more than or equal to 25%) is as follows: 0.1-0.3% of tetrasodium glutamate diacetate, 15.0-20.0% of sodium lauryl alcohol ether sulfate, 96.0-8.0% of fatty alcohol-polyoxyethylene ether, 1.0-4.0% of biodegradable nonionic surfactant, 1.0-3.0% of branched fatty alcohol alkoxy, 2.0-4.0% of cocamidopropyl betaine, 0.8-1.5% of hydrophobically modified acrylic polymer, 0.5-1.5% of gleditsia sinensis saponin, 0.05-0.07% of silicone oil emulsion, 0.1-0.3% of kasong, 0.2-0.6% of essence, 0.3-0.6% of potassium hydroxide and 1-3% of sodium chloride.

The optimal formula of the concentrated gleditschia horrida saponin laundry detergent comprises the following components: 0.2% of tetrasodium glutamate diacetate, 18.0% of sodium lauryl alcohol ether sulfate, 98.0% of fatty alcohol-polyoxyethylene ether, 2.0% of biodegradable nonionic surfactant, 4.0% of branched fatty alcohol alkoxy, 2.0% of cocamidopropyl betaine, 1.0% of hydrophobically modified acrylic polymer, 1.0% of gleditsia sinensis saponin, 0.05% of silicone oil emulsion, 0.1% of kasong, 0.3% of essence, 0.4% of potassium hydroxide and 2.2% of sodium chloride.

In the invention, the preparation method of the common type liquid soap detergent containing the gleditschia horrida saponin comprises the following steps: sequentially adding tetrasodium glutamate diacetate and sodium lauryl alcohol ether sulfate at 70-75 ℃, and stirring until the tetrasodium glutamate diacetate and the sodium lauryl alcohol ether sulfate are completely dissolved; cooling, sequentially adding fatty alcohol-polyoxyethylene ether-9, cocamide DEA and cocamidopropyl betaine, and uniformly stirring; cooling to 45 ℃, adding the pre-diluted acrylic acid homopolymer, and uniformly stirring; adding QT-182, gleditschia horrida saponin, a silicone oil defoaming agent, kasonong, sodium chloride and essence, and uniformly stirring; adding sodium hydroxide, and adjusting the pH value to about 7.5; measuring pH and viscosity, and aseptic canning.

The preparation method of the concentrated liquid laundry detergent containing the gleditschia horrida saponin comprises the following steps: completely dissolving tetrasodium glutamate diacetate, sodium dodecyl alcohol ether sulfate, fatty alcohol-polyoxyethylene ether-9, a biodegradable nonionic surfactant and branched fatty alcohol alkoxy at 70-75 ℃; cooling, sequentially adding the cocamidopropyl betaine and the hydrophobically modified acrylic polymer, and uniformly stirring; adding a proper amount of potassium hydroxide, and adjusting the pH value to 7.5; sequentially adding the gleditschia horrida saponin, the silicone oil emulsion, the kasong, the essence and the sodium chloride, and uniformly stirring; measuring pH and viscosity, and aseptic canning.

Drawings

FIG. 1 shows the result of detecting the foam height of the saponin laundry detergent of Gleditsia sinensis

FIG. 2 shows the result of the soil-removing ability test of the Gleditsia sinensis saponin laundry detergent

FIG. 3 shows the radar chart for the trial evaluation of the general type of soap pod saponin laundry detergent

FIG. 4 shows the radar chart of the trial evaluation of the concentrated type of saponin from Gleditsia sinensis

Detailed description of the preferred embodiments

Example 1 laundry detergent performance testing

Experimental methods

Height of foam

The common type and the concentrated type laundry detergent samples are respectively and uniformly mixed with water (1: 4) to obtain 20 percent liquid to be tested. And (3) sucking 1mL of liquid to be detected (20%) and adding the liquid to be detected into a test tube with scales, 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 as H, and comparing the average value with the value H, wherein the control is the liquid laundry detergent without the saponin of the gleditsia sinensis (except the saponin of the gleditsia sinensis, the other components are the same).

Soil-release capacity test

According to the following steps of 1: the normal type and the concentrated type laundry detergent are respectively prepared into 300 mL of washing liquid according to the proportion of 100. Respectively spraying artificial stains on clean cotton clothes, hemp clothes, wool clothes and synthetic fiber clothes (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 washed hair, hanging and air drying for 3 hr, and weighing to obtain hair strip m₂. The loss of soil quality was used to evaluate the detergency of the laundry detergent, and 3 parallel tests were performed to obtain an average value, and the control was a laundry detergent without the addition of saponin (the formulation was the same, and the same amount of surfactant was used instead of saponin). 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, 1mL of mouse blood and 1mL of fruit juice, and uniformly stirring the mixture by using a glass rod before each use).

1.3 results of the experiment

From the results shown in fig. 1, it can be seen that the foaming capacity and the detergency of the formula can be significantly improved by adding the saponin, the washing capacity of the traditional chemical washing and caring product can be effectively improved, and after the saponin is added, the laundry detergent obtained by the formula has good foaming capacity and detergency.

Example 2 physicochemical indices

Sensory indexes of the gleditschia horrida saponin laundry detergent are recorded through observation and trial, and comprehensive evaluation is carried out on sensory and physical and chemical properties of the gleditschia horrida saponin ordinary laundry detergent and the concentrated laundry detergent according to standards of QB/T1224-. And carrying out stability test, respectively placing the two liquid detergents at high temperature (40 +/-2 ℃) and low temperature (5 +/-2 ℃) for three months, and observing whether the two liquid detergents have layering and discoloring phenomena.

Example 3 microorganism and heavy Metal indicators

Referring to the regulations of technical Specification for safety of cosmetics (2015 edition), the microbial content and the heavy metal content of the two laundry liquids are determined according to standards of QB/T1224-.

Example 4 safety test

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。

4.1.2 Patch on skin test

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 simulation grading result of the laundry 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 purpose of the laundry detergent is to ensure the smoothness and faint scent of clothes while fully cleaning the clothes, so the specific indexes comprise: the detergent power, the mildness, the foamability, the foam abundance, the easiness in rinsing and the fragrance retention are six items. Randomly selecting 40 people, half men and women, and 20-40 years old, continuously using the self-made laundry detergent containing the gleditschia horrida saponin for five times, washing according to the same method, adding four clothes of cotton, hemp, wool and synthetic fiber which penetrate through the laundry detergent for 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 results of fig. 3 and fig. 4 show that the six indexes are good in overall performance, are consistent and positive to volunteers, and have the potential of being put into practical production and development.