High-permeability instant cationic cassia gum as well as preparation method and application thereof

Abstract

The invention discloses high-permeability instant cationic cassia gum as well as a preparation method and application thereof, and belongs to the technical field of cassia gum application, and the preparation method comprises the following steps: taking raw materials in parts by mass: dissolving neutral protease in deionized water, then adding cassia gum powder, reacting for 2-3 hours at 45-60 DEG C, and washing, filtering, drying and crushing after the reaction to obtain purified cassia gum; adding the purified gelatin into a first solvent, adding an inorganic salt, heating, adding a sodium hydroxide solid, and carrying out a heat preservation reaction for 30-60 min; adding a cationic etherifying agent, reacting for 15-30 minutes, then adding the cationic etherifying agent, reacting for 15-30 minutes, and then heating to react for 100-150 minutes; adding sodium hydroxide solid, heating to 55-65 DEG C, and reacting for 20-60 minutes; and adding acid to adjust the pH value to 7, washing, filtering, and drying to obtain the high-permeability instant cationic gelatin. The high-transparency instant cationic gelatin disclosed by the invention is high in purity and transparency, and can be applied to transparent hair washing products.

Description

Technical Field

[0001] The present invention relates to the technical field of the application of cassia gum, and particularly relates to a highly transparent and instant-soluble cationic cassia gum, a preparation method thereof and an application thereof. Background Art

[0002] At present, people's demand for improving the conditioning property in hair care product formulations is increasing. It is required that shampoos can not only provide the most basic cleaning function, but also have the effects and functions of promoting hair growth, improving scalp health, increasing hair luster, and making hair fluffy. With the continuous development of e-commerce, the demand for transparent shampoos is also increasing. The application of plant polysaccharide derivatives as thickeners, conditioners, moisturizers and antioxidants in personal care products has a long history. Cationic derivatives of guar gum and galactomannan have been successfully applied in conditioning shampoos, which can improve combability and experience. The silicone deposition performance of cationic cassia gum is better than that of other traditional cationic polymer conditioners. However, the existing cationic cassia gum solution has low transparency, which is very disadvantageous for applying cationic cassia gum as a daily chemical conditioner to transparent hair care products.

[0003] In view of the problems existing in the above-mentioned prior art, the present invention combines the design and use experience in related fields for many years, and designs a highly transparent and instant-soluble cationic cassia gum, a preparation method thereof and an application thereof to overcome the above defects. Summary of the Invention

[0004] Regarding the problems existing in the prior art, the present invention provides a highly transparent and instant-soluble cationic cassia gum, a preparation method thereof and an application thereof. The modified cationic cassia gum has the advantages of high light transmittance and low viscosity, and has unique advantages in conditioning, and can be applied to transparent shampoos.

[0005] In order to achieve the above object, the first aspect of the present invention provides a preparation method of a highly transparent and instant-soluble cationic cassia gum, including the following steps, and all the following raw materials are in parts by mass: (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, react at 45 - 60 °C for 2 - 3 h, after the reaction, wash with an aqueous alcohol solution with a mass fraction of 60 - 70%, and obtain purified cassia gum through filtration, drying and pulverization; (2) Alkalization: Add 100 - 200 parts of purified cassia gum into the first solvent, add inorganic salts, raise the temperature, and then add 20 - 40 parts of solid sodium hydroxide, and keep the temperature for reaction for 30 - 60 min to obtain a primary alkalized solution; (3) Cationic modification: Add 75 - 150 parts of cationic etherifying agent to the primary alkalized solution, react for 15 - 30 min, then add 25 - 60 parts of cationic etherifying agent, react for 15 - 30 min, and then raise the temperature and react for 100 - 150 min to obtain an etherified solution; (4) Secondary alkalization: Add 5 - 10 parts of solid sodium hydroxide to the etherification solution, heat up to 55 - 65 °C and react for 20 - 60 min to obtain the secondary alkalization solution; (5) Neutralization: After adjusting the pH of the secondary alkalization solution to 7 with acid, wash, filter, and dry to obtain the high-transparency and instant-soluble cationic cassia gum.

[0006] Preferably, in step (1), the mass ratio of cassia gum powder: deionized water: neutral protease is 1:(1.25 - 1.5):(0.005 - 0.01).

[0007] Preferably, in step (1), the aqueous alcohol solution is an ethanol aqueous solution and / or an isopropanol aqueous solution.

[0008] Preferably, in step (2), the heating temperature is 40 - 50 °C.

[0009] Preferably, in step (2), the first solvent is composed of an organic solvent and deionized water, and the organic solvent is ethanol and / or isopropanol; The organic solvent is 200 - 400 parts by mass, and the deionized water is 50 - 100 parts by mass.

[0010] Preferably, in step (2), the inorganic salt is sodium chloride and / or potassium chloride, and the inorganic salt is 3 - 6 parts by mass.

[0011] Preferably, in step (3), the heating temperature is 50 - 60 °C.

[0012] Preferably, in step (3), the cationic etherifying agent is 3-chloro-2-hydroxypropyltrimethylammonium chloride or 2,3-epoxypropyltrimethylammonium chloride; In step (5), the acid is hydrochloric acid, acetic acid, sulfuric acid or citric acid.

[0013] The second aspect of the present invention provides a high-transparency and instant-soluble cationic cassia gum prepared by the above preparation method. The transparency of the aqueous solution of the high-transparency and instant-soluble cationic cassia gum with a mass concentration of 0.5% is greater than 88%, and the viscosity of the aqueous solution of the high-transparency and instant-soluble cationic cassia gum with a mass concentration of 1% is 100 - 200 mPa·s.

[0014] The third aspect of the present invention provides an application. The high-transparency and instant-soluble cationic cassia gum prepared by the above method is applied to the field of shampoo.

[0015] The beneficial effects of the invention are as follows: 1. The present invention pre - treats the cassia gum with neutral protease, enzymatically hydrolyzes the protein - like impurities in the cassia gum into small - molecule peptide chains or amino acids, and removes them from the cassia gum by virtue of their solubility in water. At the same time, the etherified modified cassia gum is secondarily alkalized. The two together reduce the impurity content in the cassia gum, improve the transparency of the highly transparent and instant - soluble cationic cassia gum. The transparency of the aqueous solution of the highly transparent and instant - soluble cationic cassia gum with a mass concentration of 0.5% is greater than 88%, and the viscosity of the aqueous solution of the highly transparent and instant - soluble cationic cassia gum with a mass concentration of 1% is 100 - 200 mPa·s.

[0016] 2. When preparing the highly transparent and instant - soluble cationic cassia gum, the present invention adds inorganic salts, so that the highly transparent and instant - soluble cationic cassia gum can be evenly dispersed in water when used as a raw material in shampoo, avoiding agglomeration, and can be quickly dissolved after adding citric acid to obtain a transparent shampoo.

[0017] 3. The highly transparent and instant - soluble cationic cassia gum prepared by the present invention has unique advantages in conditioning. The wet - combing and dry - combing effects are better than those of cationic guar gum, and it can be applied to SLES shampoo systems and amino - acid shampoo systems. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is the flocculation effect curve graph of Test 1 - Test 4 in the present invention.

[0019] Figure 2 It is the flocculation effect curve graph of Test 5 - Test 8 in the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0020] For the convenience of those skilled in the art to understand, the present invention will be further described below in conjunction with specific embodiments.

[0021] The first aspect of the present invention provides a preparation method of a highly transparent and instant - soluble cationic cassia gum, comprising the following steps: (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, react at 45 - 60 °C for 2 - 3 h. After the reaction, wash with an alcohol aqueous solution with a mass fraction of 60 - 70%, filter, dry, and pulverize to obtain purified cassia gum. The mass ratio of cassia gum powder: deionized water: neutral protease is 1:(1.25 - 1.5):(0.005 - 0.01), and the mass ratio of cassia gum powder to the 60 - 70% alcohol aqueous solution is 1:1.5 - 2.5. The alcohol aqueous solution is preferably an ethanol aqueous solution and / or an isopropanol aqueous solution; In addition to polysaccharide polymers, cassia gum also contains impurities such as fatty acids and proteins. Direct etherification modification easily leads to low transparency of the modified cassia gum. In the present invention, neutral protease is used to enzymatically hydrolyze protein impurities into small peptide chains or amino acids. Utilizing the property that small peptide chains or amino acids are soluble in water, they are separated from the system using an alcohol aqueous solution, while retaining the polysaccharide polymers in the cassia gum, thereby improving the purity of the cassia gum. First, the neutral protease is mixed and dissolved with deionized water, and then cassia gum powder is added while controlling the ratio of deionized water to cassia gum powder, so that the cassia gum powder is in a state of water absorption and swelling, which is conducive to the full enzymatic hydrolysis reaction of the cassia gum powder.

[0022] (2) Alkalization: Add 100 - 200 parts by mass of purified cassia gum to the first solvent, add inorganic salts, heat to 40 - 50 °C, and then add 20 - 40 parts by mass of solid sodium hydroxide, and keep the temperature for reaction for 30 - 60 min to obtain a primary alkalized solution. The first solvent consists of an organic solvent and deionized water. The organic solvent is 200 - 400 parts by mass, and the deionized water is 50 - 100 parts by mass. The organic solvent is preferably ethanol and / or isopropanol. The inorganic salt is preferably sodium chloride and / or potassium chloride, and the addition amount of the inorganic salt is 3 - 6 parts by mass; (3) Cationic modification: Add 75 - 150 parts by mass of a cationic etherifying agent to the primary alkalized solution, react for 15 - 30 min, then add 25 - 60 parts by mass of a cationic etherifying agent, react for 15 - 30 min, and then heat to 50 - 60 °C and react for 100 - 150 min to obtain an etherified solution. The cationic etherifying agent is preferably 3-chloro-2-hydroxypropyltrimethylammonium chloride or 2,3-epoxypropyltrimethylammonium chloride; (4) Secondary alkalization: Add 5 - 10 parts by mass of solid sodium hydroxide to the etherified solution, heat to 55 - 65 °C and react for 20 - 60 min to obtain a secondary alkalized solution; (5) Neutralization: After adding acid to the secondary alkalized solution to adjust the pH to 7, wash, filter, and dry to obtain a highly transparent and fast-dissolving cationic cassia gum. The acid is hydrochloric acid, acetic acid, sulfuric acid, or citric acid. The present invention does not limit the concentration of the acid, aiming to adjust the pH of the secondary alkalized solution to 7.

[0023] The purified cassia gum is fully alkalized under strong alkaline conditions, providing active reaction sites for cationic etherification and facilitating the occurrence of the etherification reaction. The cationic etherifying agent is added in batches and the etherification temperature is controlled to make the etherification reaction more complete and reduce the impurities in the cassia gum. On the basis of the pretreatment with neutral protease, the present invention performs secondary alkalization after the etherification reaction, further reducing the content of impurities such as grease and cellulose in the cassia gum and significantly improving the transparency of the highly transparent and fast-dissolving cationic cassia gum.

[0024] In the second aspect of the present invention, a highly transparent and instant-soluble cationic cassia gum prepared by the above preparation method is provided. The transparency of an aqueous solution of the highly transparent and instant-soluble cationic cassia gum with a mass concentration of 0.5% is higher than 88%, and the cationic substitution degree is 0.15 - 0.25; the viscosity of an aqueous solution of the highly transparent and instant-soluble cationic cassia gum with a mass concentration of 1% is 100 - 200 mPa·s.

[0025] In the third aspect of the present invention, an application of the highly transparent and instant-soluble cationic cassia gum is provided. The above-mentioned highly transparent cationic cassia gum is used as a conditioner and applied to hair washing products, and further applied to transparent hair washing products.

[0026] In the prior art, when cationic cassia gum is used as a raw material in shampoo, it is easy to aggregate into clusters in water, prolonging the time for cationic cassia gum to disperse in water, and the transparency of cationic cassia gum is relatively low, resulting in its inability to be applied to transparent hair washing products. In the present invention, inorganic salts are added during the preparation of the highly transparent and instant-soluble cationic cassia gum to improve the dispersion degree of the highly transparent and instant-soluble cationic cassia gum in water and avoid aggregation. The highly transparent and instant-soluble cationic cassia gum can be quickly dissolved after adding citric acid.

[0027] The specific embodiments are as follows In the present invention, the nitrogen content is measured according to the test standard of GB / T 22427.10 - 2008; Transparency test method: Add 0.50 g of the final product to 99.50 g of deionized water, stir magnetically to disperse it, add 3% citric acid (based on the mass of the final product), and then stir magnetically until the viscosity is released. Keep it at a constant temperature of 25 °C for 2 h, and measure the light transmittance at 550 nm.

[0028] Viscosity measurement method: Add 1 g of the final product to 99 g of deionized water, stir magnetically to disperse it, add 3% citric acid (based on the mass of the final product), and then stir magnetically until the viscosity is released. Keep it at a constant temperature of 25 °C for 2 h, and measure the viscosity using a Brookfield viscometer. Example 1

[0029] The raw materials in the following steps are all in parts by mass (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, and react at 45 °C for 2 h. After the reaction, add 70% ethanol aqueous solution for washing. After washing twice, filter, dry, and pulverize to obtain purified cassia gum. The mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.25:0.005, and the mass ratio of cassia gum powder: ethanol aqueous solution is 1:2; (2) First alkalization: Add 100 parts of purified cassia gum to 300 parts of isopropanol and 75 parts of deionized water, add 5 parts of sodium chloride, heat up to 45 °C, and then add 25 parts of solid sodium hydroxide, and alkalize for 30 min to obtain the first alkalization solution; (3) Cationic modification: Add 75 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 30 min. Then add another 25 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 15 min. Raise the temperature to 55 °C and react for 120 min to obtain an etherification solution. (4) Secondary alkalization: Add 5 parts of solid sodium hydroxide to the etherification solution, raise the temperature to 60 °C, and react for 20 min to obtain a secondary alkalization solution. (5) Neutralization: Add 10% hydrochloric acid by mass to the secondary alkalization solution. After adjusting the pH of the solution to 7, wash, filter, and dry it with 50% ethanol aqueous solution by mass to obtain a highly transparent and fast-dissolving cationic cassia gum.

[0030] The viscosity of the 1% highly transparent and fast-dissolving cationic cassia gum aqueous solution is 136 mPa·s, the transparency of the 0.5% highly transparent and fast-dissolving cationic cassia gum aqueous solution is 89.4%, and the nitrogen content of the highly transparent and fast-dissolving cationic cassia gum is 1.69%.

[0031] This example provides a highly transparent and fast-dissolving cationic cassia gum prepared by the above preparation steps. Example 2

[0032] The raw materials in the following steps are all in parts by mass. (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, with the temperature at 45 °C and the reaction time of 2 h. After the reaction, add 70% ethanol aqueous solution for washing. After washing twice, filter, dry, and pulverize to obtain purified cassia gum, where the mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.25:0.005, and the mass ratio of cassia gum powder: ethanol aqueous solution is 1:2.

[0033] (2) Primary alkalization: Add 100 parts of purified cassia gum to 300 parts of isopropanol and 75 parts of deionized water, add 5 parts of sodium chloride, raise the temperature to 45 °C, and then add 25 parts of solid sodium hydroxide and alkalize for 30 min to obtain a primary alkalization solution.

[0034] (3) Cationic modification: Add 90 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 30 min. Then add another 60 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 15 min. Raise the temperature to 55 °C and react for 120 min to obtain an etherification solution.

[0035] (4) Secondary alkalization: Add 7 parts of solid sodium hydroxide to the etherification solution, raise the temperature to 60 °C, and react for 20 min to obtain a secondary alkalization solution.

[0036] (5)Neutralization: Add 10% hydrochloric acid by mass fraction to the secondary alkalized solution. After adjusting the pH of the solution to 7, wash, filter, and dry it with 50% ethanol aqueous solution to obtain high-transparency and instant-soluble cationic cassia gum.

[0037] The viscosity of the 1% high-transparency and instant-soluble cationic cassia gum aqueous solution is 105 mPa·s, the transparency of the 0.5% high-transparency and instant-soluble cationic cassia gum aqueous solution is 91.3%, and the nitrogen content of the high-transparency and instant-soluble cationic cassia gum is 2.5%.

[0038] This example provides a high-transparency and instant-soluble cationic cassia gum prepared by the above preparation steps. Example 3

[0039] The raw materials in the following steps are all in parts by mass (1)Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder and react at 50 °C for 2.5 h. After the reaction, add 60% ethanol aqueous solution for washing. After washing twice, filter, dry, and pulverize to obtain purified cassia gum. The mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.3:0.006, and the mass ratio of cassia gum powder: ethanol aqueous solution is 1:1.5; (2)Primary alkalization: Add 150 parts of purified cassia gum to 200 parts of ethanol and 50 parts of deionized water, add 3 parts of sodium chloride, heat up to 40 °C, and then add 20 parts of solid sodium hydroxide and alkalize for 45 min to obtain the primary alkalized solution; (3)Cationic modification: Add 75 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride to the primary alkalized solution, react for 15 min, add another 50 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 30 min, and then heat up to 50 °C and react for 100 min to obtain the etherified solution; (4)Secondary alkalization: Add 6 parts of solid sodium hydroxide to the etherified solution, heat up to 55 °C, and react for 40 min to obtain the secondary alkalized solution; (5)Neutralization: Add 5% hydrochloric acid by mass fraction to the secondary alkalized solution to adjust the pH to 7, then wash, filter, and dry with 70% ethanol aqueous solution to obtain high-transparency and instant-soluble cationic cassia gum.

[0040] The viscosity of the 1% high-transparency and instant-soluble cationic cassia gum aqueous solution is 159 mPa·s, the transparency of the 0.5% high-transparency and instant-soluble cationic cassia gum aqueous solution is 88.2%, and the nitrogen content of the high-transparency and instant-soluble cationic cassia gum is 1.4%.

[0041] This example provides a high-transparency and instant-soluble cationic cassia gum prepared by the above preparation steps. Example 4

[0042] The raw materials in the following steps are all in parts by mass. (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, and react at 60 °C for 3 h. After the reaction, add 65% isopropyl alcohol aqueous solution for washing. After washing twice, filter, dry, and pulverize to obtain purified cassia gum. The mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.5:0.01, and the mass ratio of cassia gum powder: isopropyl alcohol aqueous solution is 1:2.5.

[0043] (2) Primary alkalization: Add 200 parts of purified cassia gum to 400 parts of ethanol and 100 parts of deionized water, add 6 parts of potassium chloride, heat up to 50 °C, and then add 40 parts of solid sodium hydroxide, and alkalize for 60 min to obtain a primary alkalized solution; (3) Cationic modification: Add 150 parts of 2,3-epoxypropyltrimethylammonium chloride to the primary alkalized solution, react for 20 min, add 60 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride again and react for 20 min, and heat up to 60 °C and react for 150 min to obtain an etherified solution; (4) Secondary alkalization: Add 9 parts of solid sodium hydroxide to the etherified solution, heat up to 65 °C, and react for 60 min to obtain a secondary alkalized solution; (5) Neutralization: Add 20% sulfuric acid by mass fraction to the secondary alkalized solution, adjust the pH to 7, and then wash, filter, and dry with 50% ethanol aqueous solution by mass fraction to obtain a high-transparency and fast-dissolving cationic cassia gum.

[0044] The viscosity of a 1% high-transparency and fast-dissolving cationic cassia gum aqueous solution is 117 mPa·s, the transparency of a 0.5% high-transparency and fast-dissolving cationic cassia gum aqueous solution is 88.9%, and the nitrogen content of the high-transparency and fast-dissolving cationic cassia gum is 2.4%.

[0045] This example provides a high-transparency and fast-dissolving cationic cassia gum prepared by the above preparation steps.

[0046] Comparative Example 1 The raw materials in the following steps are all in parts by mass. (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, the temperature is 45 °C, and the reaction time is 2 h. After the reaction, add 70% ethanol aqueous solution for washing. After washing twice, filter, dry, and pulverize to obtain purified cassia gum. The mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.25:0.005, and the mass ratio of cassia gum powder: ethanol aqueous solution is 1:2.

[0047] (2) Alkalinization: Add 100 parts of purified cassia gum into 300 parts of isopropanol and 75 parts of deionized water, add 5 parts of sodium chloride, heat up to 45 °C, then add 25 parts of solid sodium hydroxide, alkalinize for 30 min, and then add another 5 parts of solid sodium hydroxide and react for 20 min; (3) Cationic modification: Add 75 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride, react for 30 min, add another 25 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride and react for 15 min, heat up to 55 °C and react for 120 min; (4) Neutralization: Adjust the pH to 7 by adding 10% hydrochloric acid by mass, then wash, filter and dry with 50% ethanol aqueous solution by mass to obtain cationic cassia gum.

[0048] The viscosity of 1% cationic cassia gum aqueous solution by mass is 183 mPa·s, the transparency of 0.5% cationic cassia gum aqueous solution by mass is 79.4%, and the nitrogen content of cationic cassia gum is 1.61%.

[0049] Comparative Example 2 The raw materials in the following steps are all in parts by mass (1) Pretreatment: Dissolve neutral protease in deionized water, then add cassia gum powder, the temperature is 45 °C, and the reaction time is 2 h. After the reaction, add 70% ethanol aqueous solution for washing, wash twice and then filter, dry and pulverize to obtain purified cassia gum, where the mass ratio of cassia gum powder: deionized water: neutral protease is 1:1.25:0.005, and the mass ratio of cassia gum powder: ethanol aqueous solution is 1:2; (2) Alkalinization: Add 100 parts of purified cassia gum into 300 parts of isopropanol and 75 parts of deionized water, add 5 parts of sodium chloride, heat up to 45 °C, then add 30 parts of solid sodium hydroxide, and alkalinize for 30 min; (3) Cationic modification: Add 100 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride, react for 45 min, heat up to 55 °C and react for 120 min; (4) Neutralization: Adjust the pH to 7 by adding 10% hydrochloric acid by mass, then wash, filter and dry with 50% ethanol aqueous solution by mass.

[0050] The viscosity of 1% cationic cassia gum by mass is 197 mPa·s, the transparency of 0.5% cationic cassia gum aqueous solution by mass is 68.6%, and the nitrogen content of cationic cassia gum is 1.53%.

[0051] Comparing Examples 1 - 4 with Comparative Example 1 and Comparative Example 2, it can be seen that through pretreatment with neutral protease and combined with secondary alkalization, the present invention greatly improves the transparency of the high - permeability and instant - soluble cationic cassia gum aqueous solution, showing synergy in the purification of cassia gum. The transparency of the aqueous solution of the high - permeability and instant - soluble cationic cassia gum with a mass concentration of 0.5% is higher than 88%. The viscosity of the aqueous solution of the high - permeability and instant - soluble cationic cassia gum with a mass concentration of 1% is 100 - 200 mPa·s. The high - permeability and instant - soluble cationic cassia gum of the present invention can be used in transparent shampoo products, while Comparative Example 1 and Comparative Example 2 cannot be used in transparent shampoo products.

[0052] Perform a shampoo formulation test on the high - permeability and instant - soluble cationic cassia gum of the present invention: 1. Take the high - permeability and instant - soluble cationic cassia gum prepared in Example 1, the high - permeability and instant - soluble cationic cassia gum prepared in Example 2, cationic guar gum C14S, and C162 as raw materials, and prepare SLES - system shampoos according to the addition amounts of each raw material in Table 1 to obtain Tests 1 - 4, and conduct a blind test on the flocculation effect and hair - bundle sensory evaluation: Table 1 Raw material ratio of SLES system Flocculation effect test: Weigh a certain amount of Tests 1 - 4 and prepare 50 - mL dilute solutions according to dilution ratios of 0, 3, 6, and 12; After stirring the diluted dilute solutions evenly into uniform liquids, use an ultraviolet - visible spectrophotometer to measure the transmittance T at a wavelength of 500 nm and plot a curve, as Figure 1 .

[0053] From Figure 1 it can be seen that when the dilution multiple is 3 times, the lower the transmittance, the better the flocculation effect. The transmittances of Tests 1 and 2 are lower than those of Tests 3 and 4, and the transmittance of Test 2 is significantly lower than that of Tests 3 and 4, indicating that the high - permeability and instant - soluble cationic cassia gum of the present invention has good flocculation characteristics in the SLES system and can effectively deposit on the hair to exert its effect.

[0054] Blind test on hair - bundle sensory evaluation (full score 10 points): 24 volunteers were recruited and randomly divided into 4 groups, with 6 people in each group. 20 standard in vitro hair bundles were randomly divided into 4 groups, with 5 bundles in each group. The 4 groups of hair bundles were smeared with the shampoo prepared in Tests 1-4 respectively. The 4 groups of volunteers conducted blind test and scoring comparison on the 4 groups of hair bundles. The 4 groups of hair bundles were rinsed and moistened with clean water. 0.5g of the shampoo prepared in Tests 1-4 was taken and evenly applied to the hair bundles. After massaging for 1 minute, the shampoo was rinsed with clean water at the same flow rate for 1 minute. The volunteers evaluated the products based on the slippery feeling of wet hair when rinsing with water, the smooth feeling of wet hair when combing, the fluffy feeling when completely dry, and the smooth feeling of dry hair. The full score is 10 points, 10 points is the best effect, the effect decreases to 8, 6, 4, 2 points, and 2 points is the worst effect. The average value is obtained in Table 2. Table 2 Sensory evaluation table of SLES system shampoo hair bundle

[0055] As can be seen from Table 2, in the SLES system, Test 1 has a good fluffy feel, and is not much different from Tests 3 and 4 in terms of wet flushing slippery feel, wet combing slippery feel, and smooth feel. Test 2 is superior to Tests 3 and 4 in terms of wet flushing slippery feel, wet combing slippery feel, and smooth feel.

[0056] 2. Take the highly permeable and fast-dissolving cationic cassia gum prepared in Example 1, the highly permeable and fast-dissolving cationic cassia gum prepared in Example 2, cationic guar gum C14S, and cationic guar gum C162 as raw materials, and prepare amino acid system shampoo according to the addition amount of each raw material in Table 3 to obtain Test 5-Test 8, and conduct blind test on flocculation effect and hair bundle sensory evaluation.

[0057] Table 3 Ratio of raw materials of amino acid system

[0058] Flocculation effect test: Weigh a certain amount of test 5 to test 8 and prepare 50 mL of dilute solution according to the dilution ratio of 0, 3, 6, and 12; After the diluted solution is stirred evenly to form a uniform liquid, the transmittance T at a wavelength of 500nm is tested using a UV-visible spectrophotometer and a curve is drawn, such as Figure 2 shown.

[0059] from Figure 2 It can be seen that when the dilution factor is 3 times, the transmittance of test 5 and test 6 is significantly lower than that of test 7 and test 8, indicating that the highly permeable and fast-dissolving cationic cassia gelatin of the present invention also has unique flocculation properties in the amino acid system and can be effectively deposited on the hair to exert its effect.

[0060] Hair bundle sensory evaluation blind test (full score 10 points): 24 volunteers were recruited and randomly divided into 4 groups, with 6 people in each group. 20 standard in vitro hair bundles were randomly divided into 4 groups, with 5 bundles in each group. The 4 groups of hair bundles were rinsed and moistened with clean water. The 4 groups of hair bundles were smeared with the shampoo prepared in Tests 5-8 respectively. The 4 groups of volunteers conducted a blind test and scored comparison on the 4 groups of hair bundles. 0.5g of the shampoo prepared in Tests 5-8 was taken and evenly applied to the hair bundles respectively. After massaging for 1 minute, the hair bundles were rinsed with clean water at the same flow rate for 1 minute. The volunteers evaluated the products based on the slippery feeling of wet hair when rinsing with water, the smooth feeling of wet hair when combing, the fluffy feeling when completely dry, and the smooth feeling of dry hair. The full score is 10 points, 10 points is the best effect, the effect decreases to 8, 6, 4, 2 points, and 2 points is the worst effect. The average value is obtained in Table 4; Table 4 Sensory evaluation table of amino acid system shampoo hair bundle

[0061] As can be seen from Table 4, in the amino acid system, test 5 has a good fluffy feeling, and is not much different from test 7 and test 8 in terms of wet flushing slippery feeling, wet combing slippery feeling, and smooth feeling. Test 6 has better wet and dry smooth feeling and good wet flushing property. Tables 2 and 4 show that the highly permeable and fast-dissolving cationic cassia gelatin prepared by the present invention has a good wet and dry combing effect, and can be used as a conditioning agent in SLES system and amino acid system shampoo.

[0062] It should be understood that the purpose of these embodiments is only to illustrate the present invention and is not intended to limit the protection scope of the present invention. In addition, it should also be understood that after reading the technical content of the present invention, those skilled in the art can make various changes, modifications and / or variations to the present invention, and all of these equivalent forms also fall within the protection scope defined by the claims attached to this application.

Claims

1. A method for preparing a highly permeable and fast-dissolving cationic cassia gelatin, characterized in that: The process comprises the following steps, wherein the following raw materials are measured by weight: (1) Pretreatment: Dissolve neutral protease in deionized water, then add Cassia gelatin powder, react at 45-60°C for 2-3h, wash with 60-70% alcohol aqueous solution after the reaction, filter, dry and grind to obtain purified Cassia gelatin; (2) Alkalization: add 100-200 parts of purified cassia gelatin to the first solvent, add inorganic salt, add 20-40 parts of solid sodium hydroxide after heating, and keep the temperature to react for 30-60 minutes to obtain a primary alkalized solution; (3) Cationic modification: add 75-150 parts of cationic etherifying agent to the primary alkalized solution, react for 15-30 minutes, then add 25-60 parts of cationic etherifying agent, react for 15-30 minutes, and then heat and react for 100-150 minutes to obtain an etherified solution; (4) Secondary alkalization: add 5-10 parts of sodium hydroxide solid to the etherified liquid, raise the temperature to 55-65°C and react for 20-60 minutes to obtain a secondary alkalized liquid; (5) Neutralization: After adding acid to the secondary alkalized liquid to adjust the pH to 7, wash, filter and dry to obtain highly permeable and fast-dissolving cationic Cassia gelatin.

2. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: In step (1), the mass ratio of Cassia gelatin powder: deionized water: neutral protease is 1: (1.25-1.5): (0.005-0.01).

3. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: The alcohol aqueous solution in step (1) is an ethanol aqueous solution and / or an isopropanol aqueous solution.

4. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: The heating temperature in step (2) is 40-50°C.

5. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: In step (2), the first solvent consists of an organic solvent and deionized water, and the organic solvent is ethanol and / or isopropanol; The organic solvent is 200-400 parts by mass, and the deionized water is 50-100 parts by mass.

6. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: The inorganic salt in step (2) is sodium chloride and / or potassium chloride, and the inorganic salt is 3-6 parts by weight.

7. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: The heating temperature in step (3) is 50-60°C.

8. The method for preparing a highly permeable and fast-dissolving cationic cassia gelatin according to claim 1, characterized in that: In step (3), the cationic etherifying agent is 3-chloro-2-hydroxypropyltrimethylammonium chloride or 2,3-epoxypropyltrimethylammonium chloride; In step (5), the acid is hydrochloric acid, acetic acid, sulfuric acid or citric acid.

9. A highly permeable and fast-dissolving cationic cassia gelatin, characterized in that: The highly permeable and fast-dissolving cationic Cassia gelatin is prepared by the preparation method described in any one of claims 1 to 8. The transparency of the aqueous solution of the highly permeable and fast-dissolving cationic Cassia gelatin with a mass concentration of 0.5% is greater than 88%, and the viscosity of the aqueous solution of the highly permeable and fast-dissolving cationic Cassia gelatin with a mass concentration of 1% is 100 to 200 mPa.s.

10. An application of a highly permeable and fast-dissolving cationic cassia gelatin, characterized in that: The highly permeable and fast-dissolving cationic cassia gelatin described in claim 9 is used as a conditioning agent in transparent shampoo products.

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