Hydrogenated castor oil suspending agent, microcapsule essence gel bead containing hydrogenated castor oil suspending agent and preparation method of microcapsule essence gel bead

Abstract

The invention discloses a hydrogenated castor oil suspending agent, microcapsule essence gel beads containing the hydrogenated castor oil suspending agent and a preparation method of the microcapsule essence gel beads, and belongs to the technical field of daily chemical products. According to the invention, the hydrogenated castor oil suspending agent is obtained by selecting components in a proper mass part range and a proper preparation method, and then the hydrogenated castor oil suspending agent is compounded with components in a specific mass part range; according to the microcapsule essence gel bead, good shelf life stability and excellent dirt-removing power of the microcapsule essence gel bead can be realized on the basis of realizing an excellent fragrance retaining effect by adding a relatively high content of microcapsule essence.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of daily chemical products, and particularly relates to a hydrogenated castor oil suspending agent, a microcapsule fragrance condensation bead containing the same, and a preparation method thereof. BACKGROUND

[0002] In the field of washing products, consumers list "long-lasting fragrance of clothes" and "rich and layered fragrance" as key factors for purchasing fabric washing products, which are also the main factors for the current popularity of fragrance beads / microcapsule fragrance (liquid) condensation beads. In the current market, the total amount of microcapsule fragrance added in the fragrance beads / microcapsule fragrance (liquid) laundry condensation beads is generally less than 5%, such as patent CN108893212A which introduces a laundry condensation bead with a microcapsule fragrance addition amount of 0.1-0.6% and a preparation method thereof. In the case of low microcapsule fragrance content, the fragrance perception of consumers will be significantly weaker, and the long-lasting fragrance effect of clothes will also be compromised.

[0003] When the solid fragrance beads are added to the condensation beads, the production efficiency in the workshop will be significantly reduced due to the inconsistency of the solid-liquid flow rate and the filling process, such as the fragrance beads added in the condensation bead liquid described in patent CN213012733U which may also have a certain impact on the stability of the liquid detergent. The microcapsule fragrance is suspended in the condensation bead in the form of a liquid by using a suspending agent, which has no significant impact on the stability of the detergent, but as described in patent CN113817549B, the microcapsule added in the condensation bead is prone to automatic aggregation, resulting in visible gelatinous aggregates in the condensation bead, which seriously affects the appearance quality of the condensation bead and the fragrance retention time and concentration of the fragrance microcapsule.

[0004] At the same time, the compatibility between the microcapsule and the system components (such as solvents and surfactants) is poor, and sedimentation or rupture is also prone to occur. For example, due to the large steric hindrance and charge shielding effect of PEG solvents, the microcapsule fragrance cannot be uniformly dispersed, resulting in aggregation of the microcapsule fragrance in the system. High content of microcapsule fragrance is often accompanied by high addition amount of suspending agent, which will significantly increase the viscosity of the system, and even cause gelation of the condensation bead system under high temperature for a short period of time or at room temperature for a long period of time. SUMMARY

[0005] The present application aims to overcome the shortcomings of the prior art and provide a hydrogenated castor oil suspending agent with a high content of microcapsule fragrance, long-lasting fragrance retention capability, low viscosity, and excellent shelf stability and decontamination capability, a microcapsule fragrance condensation bead containing the same, and a preparation method thereof.

[0006] To achieve the above-mentioned purpose, in the first aspect of the present application, the present application provides a hydrogenated castor oil suspending agent, which comprises the following components by mass percentage: Sodium linear alkylbenzene sulfonate 18-22%, sodium fatty alcohol polyoxyethylene ether sulfate 0.1-3%, lauric acid 0.1-2%, monoethanolamine 0.1-0.3%, hydrogenated castor oil 8-12%, pH adjuster 1-3%, water balance.

[0007] This invention has found that by selecting and compounding the above-mentioned types of components, the stability of the microcapsule flavor beads system can be effectively improved by the subsequent hydrogenated castor oil suspension.

[0008] In one embodiment, the pH adjuster includes at least one of sodium hydroxide and sodium citrate.

[0009] In a second aspect, the present invention provides a method for preparing the hydrogenated castor oil suspension, the method comprising the following steps: (1) Sodium linear alkylbenzene sulfonate and dodecanoic acid were added to a portion of water, followed by the addition of monoethanolamine and pH adjuster to make the pH of the system 6-8. Then, sodium fatty alcohol polyoxyethylene ether sulfate was added and heated to 85-90℃. Hydrogenated castor oil (HCO) was added to dissolve and homogenized to obtain an O / W emulsion. (2) Add the remaining water to the O / W emulsion and homogenize it. Then cool it to 55-65℃ and keep it at that temperature for 0.5-1h. After the temperature is kept at that temperature, cool it to 50±2℃ at a cooling rate of 0.5-1.5℃ / min. Then turn off the homogenizer and turn on the stirring. Then cool it to below 40℃ to obtain hydrogenated castor oil suspension.

[0010] This invention has found that the preparation method provided by this invention can better form hydrogenated castor oil suspension with β-crystal as the main crystal, thereby effectively increasing the yield stress of the hydrogenated castor oil suspension, improving its suspension effect on microcapsule flavors, and thus improving the shelf-life stability of the microcapsule flavor beads prepared subsequently.

[0011] Specifically, in step (1), HCO exhibits better emulsification in a system primarily composed of linear alkylbenzene sulfonate and supplemented by dodecanoic acid and fatty alcohol polyoxyethylene ether sulfate. HCO reaches its melting point within the 85-90℃ range, transforming from a solid to a liquid and emulsifying within the system. Further, the homogeneous shearing action disperses the molten HCO into smaller oil droplets within the emulsion. Then, through heat preservation within a specific temperature and time range in step (2), and cooling at a specific rate after heat preservation, HCO can generate crystals with a higher β-crystal form during secondary crystallization, resulting in lower shear viscosity values. Subsequent addition to the bead system can achieve higher yield stress. The applicant speculates that the reason is: when HCO melts in an aqueous emulsion system containing surfactants, flocculation and aggregation dominate the emulsion instability process at low shear rates; flocculation originates from the dual effects of van der Waals attraction and electrostatic repulsion; during flocculation, a distance still exists between oil droplets, which depends on the overall interfacial potential, thus maintaining the integrity of the droplet structure. Coagulation, on the other hand, breaks down the energy barrier between droplets, allowing small droplets to gradually aggregate into larger clumps. As the shear rate increases, the shear force surpasses the flocculation and coalescence effects, causing the droplets to break down into even smaller and more uniformly sized droplets. Homogeneity provides a higher shear rate than ordinary stirring, enabling HCO3- to disperse in the emulsion as smaller oil droplets, thus preventing the formation of irregular crystals during subsequent secondary crystallization.

[0012] In one embodiment, in step (1), the homogenization frequency is 20-50Hz and the homogenization time is 20-40min.

[0013] In one embodiment, in step (2), the homogeneous frequency is 20-50Hz.

[0014] In one embodiment, in step (2), the stirring speed is 150-300 rpm and the stirring time is 30-60 min.

[0015] The present invention has found that when the homogenization and stirring parameters are further selected within the above range, the resulting hydrogenated castor oil suspension has a higher yield stress and a better subsequent suspension effect on microcapsule flavorings, thereby effectively improving the shelf-life stability, fragrance retention, and stain resistance of microcapsule flavoring beads.

[0016] A third aspect of the invention provides the application of the hydrogenated castor oil suspension in the preparation of microcapsule flavor beads.

[0017] The hydrogenated castor oil suspending agent provided by this invention has excellent stability and high yield stress, which can effectively suspend microcapsule particles, and thus can be widely used in the preparation of microcapsule fragrance beads; the obtained microcapsule fragrance beads have excellent shelf-life stability, long-lasting fragrance retention and excellent detergency.

[0018] A fourth aspect of the present invention provides microcapsule flavor beads, the microcapsule flavor beads comprising a core and a coating layer, the core comprising a bead composition, the bead composition comprising the following components in weight percentages: The hydrogenated castor oil suspension contained in this application is 8-16%, anionic surfactant is 20-28%, nonionic surfactant is 10-16%, microencapsulated flavor is 6-10%, polymer is 0.1-5%, monoethanolamine is 3.5-6%, functional additives are 0-1%, and the balance is C3-C6 polyhydroxy alcohol. The anionic surfactants include sulfonate anionic surfactants; The nonionic surfactant includes isomeric fatty alcohol alkoxylates; The C3-C6 polyhydroxy alcohols include propylene glycol and glycerol; The polymer includes a cationic acrylamide polymer.

[0019] The present invention has found that when the above-mentioned substances are compounded within a specific mass percentage range, and the mass percentage of added microcapsule fragrance reaches 6-10%, the resulting gel bead composition has a suitable viscosity. At the same time, the resulting microcapsule fragrance gel beads also have good shelf-life stability, long-lasting fragrance retention, and excellent stain resistance.

[0020] Specifically, firstly, increasing the concentration of nonionic surfactant within a certain range leads to the formation of numerous micelles. These micelles create a "depletion zone" around the microcapsules, resulting in an osmotic pressure difference between the microcapsules, causing them to approach and aggregate (similar to the phenomenon of "depletion flocculation"), thus making the system unstable. Conversely, if the nonionic surfactant content is too low, the solubilizing effect of the system on the microcapsule fragrance will deteriorate, leading to microcapsule precipitation during long-term storage, i.e., a significant decrease in shelf-life stability. Therefore, this invention selects the mass percentage of nonionic surfactant within a certain range to achieve a good overall effect for the product. Secondly, selecting the mass percentage of microcapsule fragrance within a certain range ensures both long-lasting fragrance and good shelf-life stability of the system.

[0021] In one embodiment, the anionic surfactant further includes at least one of fatty acid salts, fatty alcohol polyether sulfates, and modified oil ethoxylate sodium sulfonate.

[0022] For example, the fatty acid salt includes at least one of coconut oil fatty acid salt, laurate, and stearate.

[0023] For example, the fatty alcohol polyether sulfate includes at least one of sodium fatty alcohol polyoxyethylene ether sulfate (AES), ammonium fatty alcohol polyoxyethylene ether sulfate (AESA), and sodium lauryl polyoxyethylene ether sulfate (SLES).

[0024] This invention has found that when the above-mentioned type of anionic surfactant is further introduced into the system, it can interact with sulfonate anionic surfactants, thereby improving the shelf-life stability of the product.

[0025] In one embodiment, the nonionic surfactant further includes at least one of fatty alcohol alkoxylates, fatty acid ester ethoxylates, oil ethoxylates, and fatty alcohol amide ethoxylates.

[0026] In one embodiment, the C3-C6 polyhydroxy group further includes at least one of isopropanol, 1,3-butanediol, erythritol, xylitol, sorbitol, and isohexyldiol.

[0027] In one embodiment, the polymer further includes polyethyleneimine ethoxylate.

[0028] This invention has found that the addition of polyethyleneimine ethoxylate can work together with cationic acrylamide polymer and isomeric fatty alcohol alkoxylate to effectively improve the dispersion uniformity of microcapsule fragrances, maintain the viscosity of the system within a suitable range, and thus improve the anti-fouling effect, long-lasting fragrance ability and shelf-life stability of microcapsule fragrances.

[0029] In one embodiment, the functional additive includes at least one of pigments, opacifiers, and bioenzymes.

[0030] For example, the light-blocking agent may be a silicone light-blocking agent, such as OP 301.

[0031] For example, the bioenzyme includes at least one of protease, cellulase, and amylase.

[0032] In one embodiment, the sulfonate anionic surfactant comprises 65-90% by mass of the anionic surfactant.

[0033] This invention has discovered that the -SO3H groups of sulfonic acid in sulfonate anionic surfactants can form hydrogen bonds or ion-dipole interactions with 12-hydroxystearic acid microcrystals of HCO, thereby forming a three-dimensional network structure. Simultaneously, the rigid structure of sulfonic acid micelles can serve as nucleation sites, promoting the orderly arrangement of HCO microcrystals and forming a gel network. Therefore, sulfonate anionic surfactants not only affect the suspension and dispersion stability of microcapsule fragrances but also influence the degree of gelation in the system. When the mass percentage of sulfonate anionic surfactants in the anionic surfactant is further selected within the aforementioned range, the resulting microcapsule fragrance beads maintain good long-lasting fragrance retention while also exhibiting excellent detergency and shelf-life stability.

[0034] In one embodiment, the mass percentage of the isomeric fatty alcohol alkoxylate is 10-50% based on the mass of the nonionic surfactant.

[0035] This invention has found that the addition of isomeric fatty alcohol alkoxylates can reduce the viscosity of the system to a certain extent, while shielding some micelle electrostatic interactions within the system and influencing the proximity between micelles or microcapsules through steric hindrance. This reduces the system viscosity, improves the dispersion uniformity of microcapsule fragrances, and prevents gelation during the shelf life, thus reducing shelf-life stability. In particular, when the mass percentage of isomeric fatty alcohol alkoxylates in the nonionic surfactant is further selected to be 10-50%, the resulting microcapsule fragrance beads exhibit even better overall performance.

[0036] In one embodiment, the cationic acrylamide polymer has a mass percentage of 9-46% based on the mass of the polymer.

[0037] This invention has found that selecting a cationic acrylamide polymer as the polymer can form uneven positively charged patches on the surface of microcapsule fragrances through its long-chain structure, thereby enhancing the dispersibility and uniformity of the microcapsule fragrances through local electrostatic repulsion. Simultaneously, it also has a certain influence on the viscosity of the system. Therefore, when the mass percentage of the cationic acrylamide polymer in the polymer is further selected to be 9-46%, the resulting microcapsule fragrance beads exhibit superior overall performance.

[0038] In one embodiment, the propylene glycol comprises 5-18% by mass and the glycerin comprises 15-30% by mass, based on the total mass of the microcapsule flavor beads composition.

[0039] This invention has found that both propylene glycol and glycerin can achieve good dispersibility in the system and have a good pre-dispersion effect on microcapsule flavors. In particular, when the mass percentages of propylene glycol and glycerin in the system are within the above-mentioned range, the overall performance of the obtained product is even better.

[0040] In one embodiment, the sulfonate anionic surfactant includes at least one of linear alkylbenzene sulfonates and alkyl sulfonates.

[0041] This invention has found that when the above-mentioned types of sulfonate anionic surfactants are selected, the resulting products have better overall performance.

[0042] In one embodiment, the isomeric fatty alcohol alkoxylate includes at least one of isomeric AEO 7, the product of the polymerization reaction of isomeric C9-C11 alcohol with ethylene oxide, and the product of the polymerization reaction of isomeric C9-C11 alcohol with a mixture of ethylene oxide and propylene oxide.

[0043] This invention has found that when selecting the above-mentioned types of isomeric fatty alcohol alkoxylates, the resulting products have better overall effects.

[0044] In one embodiment, the coating layer includes a water-soluble film, which includes any one of polyvinyl alcohol film, starch film, gelatin film, and polyvinyl acid film.

[0045] A fifth aspect of the present invention provides a method for preparing the aforementioned microcapsule flavor beads, the method comprising the following steps: (1) A portion of C3-C6 polyhydroxy alcohols were mixed with hydrogenated castor oil suspending agent to obtain premix A; (2) Mix another portion of C3-C6 polyhydroxy alcohol with anionic surfactant and nonionic surfactant to obtain premix B; (3) Mix the remaining C3-C6 polyhydroxy alcohol with the microcapsule flavoring to obtain premix C; (4) After adjusting the pH of premix B to 7.5-8.5 and the temperature to 20-45℃, add premix A and stir for the first time, then add premix C and stir for the second time, then stir for the third time and add polymer and functional additives in sequence to obtain microcapsule flavor beads composition. (5) After vacuuming the microcapsule flavor gel beads composition, it is coated with a coating layer to obtain microcapsule flavor gel beads.

[0046] This invention has found that by using the above-mentioned preparation method, the problems of poor dispersion caused by polarity differences between substances and the inability of substances to interact effectively to form a three-dimensional network structure, thus reducing the suspension ability of microcapsule flavorings, can be effectively reduced.

[0047] In one embodiment, in step (1), the mass ratio of a portion of the C3-C6 polyhydroxy alcohol to the hydrogenated castor oil suspending agent is greater than or equal to 1.

[0048] In one embodiment, in step (1), the mass ratio of a portion of the C3-C6 polyhydroxy alcohol to the hydrogenated castor oil suspending agent is 1-1.5.

[0049] In one embodiment, in step (3), the mass ratio of the remaining C3-C6 polyhydroxy alcohol to the microcapsule flavor is greater than or equal to 1.

[0050] In one embodiment, in step (3), the mass ratio of the remaining C3-C6 polyhydroxy alcohol to the microcapsule flavor is 1-1.5.

[0051] The present invention has found that dispersing hydrogenated castor oil suspension with a portion of C3-C6 polyhydroxy alcohol in step (1) and dispersing microcapsule flavor in step (3) can effectively improve the dispersion uniformity of premix A and premix C in premix B, thereby improving the shelf life stability of the product.

[0052] In one embodiment, the first stirring speed is 400-700 rpm, and the first stirring time is 5-20 min.

[0053] In one embodiment, the second stirring speed is 400-700 rpm, and the second stirring time is 5-20 min.

[0054] In one embodiment, the third stirring speed is 400-700 rpm, and the third stirring time is 10-30 min.

[0055] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention obtains hydrogenated castor oil suspension by selecting components within a suitable mass range and using a suitable preparation method. Subsequently, it is compounded with components within a specific mass range. This not only achieves excellent fragrance retention by adding a high content of microcapsule fragrance, but also achieves good shelf-life stability of microcapsule fragrance beads and excellent detergency. Attached Figure Description

[0056] Figure 1 This is a microstructure diagram of hydrogenated castor oil suspension 1; Figure 2 This is a microstructure diagram of hydrogenated castor oil suspension 3. Detailed Implementation

[0057] To better illustrate the purpose, technical solution, and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0058] Unless otherwise specified, the reagents, methods and equipment used in this invention are all conventional reagents, methods and equipment in the field; and unless otherwise specified, the raw materials used in parallel experiments are from the same batch.

[0059] Hydrogenated castor oil suspension 1: includes 18% sodium linear alkylbenzene sulfonate (LAS), 0.5% sodium fatty alcohol polyoxyethylene ether sulfate (AES), 8% hydrogenated castor oil, 0.2% monoethanolamine, 0.5% dodecanoic acid, appropriate amount of pH adjuster, and water to make up to 100%. The preparation method of the hydrogenated castor oil suspension 1 includes the following steps: LAS and lauric acid are added to a portion of water (accounting for 50% of the total water), and pH adjuster (NaOH and sodium citrate) and monoethanolamine are added sequentially. The mixture is stirred until the pH value of the system is 7. Then, AES is added, and the temperature is heated to 85-90℃. Solid HCO3 is added, and after the HCO3 is completely dissolved, homogenization is started (homogenization frequency is 40Hz, homogenization time is 30min) to fully disperse the HCO3 and form an O / W emulsion. Then, the remaining water is added and homogenized (homogenization speed is 40rpm, homogenization time is 30min). Then, the temperature is lowered to 60±5℃ and kept at this temperature for 45min. After the holding time is completed, the temperature is lowered to 50±2℃ at a cooling rate of 0.5-1.5℃ / min. Homogenization is stopped and stirring is started (stirring speed is 200rpm, stirring time is 45min). The temperature is then lowered to 40℃ to obtain hydrogenated castor oil suspension 1.

[0060] Hydrogenated castor oil suspension 2: The difference between this and hydrogenated castor oil suspension 1 is that it includes 22% sodium linear alkylbenzene sulfonate (LAS), 3% sodium fatty alcohol polyoxyethylene ether sulfate (AES), 10% hydrogenated castor oil, 0.2% monoethanolamine, 2% lauric acid, appropriate amount of pH adjuster, and water to make up to 100%.

[0061] Hydrogenated castor oil suspension 3: consists of 20% sodium fatty alcohol polyoxyethylene ether sulfate (AES), 8% hydrogenated castor oil, and the remainder water to make up to 100%; The preparation method of the hydrogenated castor oil suspension 3 includes the following steps: AES is added to a portion of deionized water (accounting for 60% of the total deionized water), heated to a temperature of 85-90℃, and then solid HCO is added. After the HCO is completely dissolved, homogenization is started (homogenization frequency is 40Hz, homogenization time is 30min) to fully disperse the HCO and form an O / W emulsion; then the remaining water is added and homogenized (homogenization speed is 40rpm, homogenization time is 30min); then the temperature is lowered to 60±5℃ and kept at that temperature for 45min. After the holding time is completed, the temperature is lowered to 50±2℃ at a cooling rate of 0.5-1.5℃ / min, homogenization is stopped and stirring is started (stirring speed is 200rpm, stirring time is 45min), and the temperature is further lowered to 40℃ to obtain hydrogenated castor oil suspension 3.

[0062] Hydrogenated castor oil suspension 4: consists of 10% sodium fatty alcohol polyoxyethylene ether sulfate (AES), 20% AEO-9, 20% glycerin, and the balance propylene glycol to bring the total to 100%. The preparation method of the hydrogenated castor oil suspension 4 includes the following steps: AES and AEO-9 are added to a portion of propylene glycol (accounting for 50% of the total propylene glycol), heated to a temperature of 85-90℃, and then solid HCO is added. After the HCO is completely melted, homogenization is started (homogenization frequency is 40Hz, homogenization time is 30min) to fully disperse the HCO and form an O / W emulsion; then the remaining portion of propylene glycol is added and homogenized (homogenization speed is 40rpm, homogenization time is 30min); then the temperature is lowered to 60±5℃ and held for 45min. After the holding time is completed, the temperature is lowered to 50±2℃ at a cooling rate of 0.5-1.5℃ / min, homogenization is stopped and stirring is started (stirring speed is 200rpm, stirring time is 45min), and the temperature is further lowered to 40℃ to obtain hydrogenated castor oil suspension 4.

[0063] The microstructure of hydrogenated castor oil 1-4 was observed using an Olympus microscope in dark field. Specifically, the crystals of hydrogenated castor oil suspensions 1-2 exhibited needle-like cross-shaped and needle-like linear patterns, while the crystals of hydrogenated castor oil suspensions 3-4 showed small-particle cross-shaped patterns. The microstructure of hydrogenated castor oil suspension 1 is shown in the image below. Figure 1 As shown, the microstructure diagram of hydrogenated castor oil suspension 3 is as follows. Figure 2 As shown.

[0064] Examples 1-21 and Comparative Examples 1-13 The present invention provides a microcapsule fragrance granule, comprising a core and a coating layer, wherein the core comprises a granule composition, and the granule composition comprises the following component contents (mass percentages) as shown in Tables 1-3; Table 1 Table 2 Table 3 The preparation method of the microcapsule fragrance beads provided in Example 1 is as follows: (1) After mixing anionic surfactant, nonionic surfactant, C3-C6 polyhydroxy alcohol and monoethanolamine evenly, adjust the pH of the system to about 8 and keep the temperature below 45℃ to form mixture B; (2) Add hydrogenated castor oil suspending agent and part of C3-C6 polyhydroxy alcohol pre-dispersed according to the formula ratio, and stir evenly; (3) Add microcapsule flavor and part of C3-C6 polyhydroxy alcohol pre-dispersed according to the formula ratio of premix C, and stir evenly; (4) Add premix A to premix B and stir for the first time (stirring speed is 600 rpm, stirring time is 15 min), then add premix C and stir for the second time (stirring speed is 600 rpm, stirring time is 15 min), then stir for the third time (stirring speed is 600 rpm, stirring time is 25 min), and then add polymer and functional additives in sequence to obtain microcapsule flavor granule composition; (5) After vacuum degassing the microcapsule flavor beads composition, the beads are coated with polyvinyl alcohol film to obtain microcapsule flavor beads.

[0065] The preparation methods of the microcapsule fragrance beads provided in Examples 2-21 and Comparative Examples 1-13 are consistent with those in Example 1, except that the relevant components are not required.

[0066] Example 1 The performance of the microcapsule flavor beads prepared in the present invention's efficacy examples and comparative examples includes the following aspects: 1. Yield stress test: The test was conducted using a Brookfield RST rheometer at a temperature of 25°C, with a shear rate scan range of 0.01–100 s. -1 , from 0.1 to 100 s -1 The data were fitted using the Herschel-Bulkley model, with a stability index R² greater than 0.999. The test samples were initial samples (samples that had not been stored for a long time under conditions such as high temperature).

[0067] 2. Viscosity test: After the sample is kept at a constant temperature of 25°C, it is tested using an NDJ-1B rotational viscometer. The test sample is the initial sample (the sample has not been stored under high temperature or other conditions for a long time, and the test beads composition is tested).

[0068] 3. Stability Test: Place the relevant samples under appropriate conditions and observe whether there are unstable phenomena such as stratification, microcapsule aggregation and sedimentation (test at 50℃ for one month, and at 45℃ and room temperature for two months); where the room temperature is 25℃ (×: there are unqualified appearance phenomena such as stratification of beads and aggregation of microcapsules; √: the appearance test is qualified; slight gel: the beads have poor fluidity and flow slowly; gel: the beads do not flow or hardly flow), and record the number of days when unstable phenomena occur at -5℃.

[0069] 4. Fragrance retention strength test method: Towels were washed with a concentration of 0.5g / L in a washing machine. After washing, 15 evaluators were randomly selected to score the fragrance retention strength of the towels (evaluation after rubbing). Specifically, after hand-rubbing the washed towels 3-4 times, the evaluators smelled all the towels through their nasal cavity and gave a score. The score between samples was based on a 7-point scale. At the same time, two commercially available products were introduced into the fragrance retention strength test. Commercially available product 1 did not contain microcapsule fragrance, and commercially available product 2 contained only a small amount of microcapsule fragrance (accounting for ≤1%).

[0070] 5. Stain removal test method: The stain removal power test shall be conducted in accordance with GB / T13174 "Determination of stain removal power and recycle washing performance of detergents for clothing", and the ratio of the stain removal value of carbon black oil stains to the stain removal value of standard laundry detergent shall be calculated.

[0071] If the stability is not up to standard, the fragrance retention strength and stain removal ability will not be tested; the results of the above tests are shown in Table 4. Table 4 As can be seen from Table 4, when the technical solution of the present invention is adopted, the obtained product has high yield stress, suitable viscosity range, good stability, rich and long-lasting fragrance, and good detergency. Specifically, the yield stress of the obtained product is above 0.72 Pa, the viscosity is between 747-958 mPa·s, no layering or gelation occurs at three temperatures in the stability test, the stability days at -5℃ are above 3 days, the immediate fragrance score is above 6 points, the fragrance score after 120 hours is above 5.7 points, and the ratio in the detergency test is above 1. As can be seen from Example 1 and Comparative Examples 1-2, the amount of nonionic surfactant added affects the yield stress, viscosity and stability of the obtained product. When the amount of nonionic surfactant added in Comparative Example 1 is too large, the viscosity and yield stress of the obtained product decrease significantly, and stratification occurs in the stability test. When the mass percentage of nonionic surfactant in Comparative Example 2 is too small, the viscosity of the obtained product increases significantly, and gelation or slight gelation occurs in the stability test. As can be seen from Example 1 and Comparative Examples 3-4, the amount of anionic surfactant added affects the overall performance of the product. When the mass percentage of anionic surfactant in Comparative Example 3 is too high, the viscosity of the obtained product increases significantly, and obvious gelation occurs in the stability test, indicating that the stability is not up to standard. When the mass percentage of anionic surfactant in Comparative Example 4 is too low, the yield stress of the obtained product decreases significantly, the viscosity decreases significantly, and stratification occurs in the stability test. Moreover, the retention time at -5°C is only 1 day. As can be seen from Examples 1 and Comparative Examples 5-6, the amount of hydrogenated castor oil suspending agent added affects the overall performance of the product. When the mass percentage of hydrogenated castor oil suspending agent in Comparative Example 5 is too low, the yield stress of the obtained product decreases significantly, the viscosity decreases significantly, and stratification occurs in the stability test. Moreover, the product only maintains its stability at -5°C for 1 day. When the mass percentage of hydrogenated castor oil suspending agent in Comparative Example 6 is too high, the viscosity of the obtained product increases significantly, gelation or slight gelation occurs in the stability test, and the stability at -5°C also decreases significantly. As can be seen from Example 1 and Comparative Example 7, when the mass percentage of the polymer in Comparative Example 7 is not within the range given in this invention, specifically, when the amount added is too much, the resulting product will show stratification in the stability test, and the number of days it can be maintained at -5°C is only 1 day. As can be seen from Examples 1 and 8, when no sulfonate anionic surfactant is added, the resulting products exhibit stratification in stability tests, and the retention time at -5°C is only 1 day. As can be seen from Examples 1 and 9, when no isomeric fatty alcohol alkoxylate is added, although the resulting products show relatively excellent stability at -5°C, gelation or slight gelation occurs in stability tests at the other three temperatures. As can be seen from Examples 1 and 10, when no cationic acrylamide polymer is added, the resulting products have poor high-temperature stability (45°C and 50°C), exhibiting stratification in stability tests. As can be seen from Examples 1 and 11, when the hydrogenated castor oil suspending agent and microcapsule flavor are not premixed with the solvent during preparation, the yield stress of the resulting products decreases significantly, and the stability at various temperatures also decreases significantly. As can be seen from Examples 1 and 12-13, when the hydrogenated castor oil suspending agent is not the technical solution of this invention, the stability of the resulting products decreases significantly.

[0072] Example 3 The shelf-life stability of the microcapsule flavor beads prepared in Example 1 was verified by the present invention, and the results are shown in Table 5. Table 5 Group Room temperature for one year Room temperature for one and a half years Bead appearance Pass Pass Linger strength 6.5 6.3 Detergency (carbon black stained cloth) 1.03 1.05 As can be seen from Table 5, the results of the long-term shelf-life performance tracking study show that the microcapsule flavor beads prepared by the process and formula of this invention can be stored within the shelf life, and have good appearance stability, fragrance retention strength and stain removal performance.

[0073] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A hydrogenated castor oil suspension, characterized in that, The hydrogenated castor oil suspension comprises the following components by mass percentage: Sodium linear alkylbenzene sulfonate 18-22%, sodium fatty alcohol polyoxyethylene ether sulfate 0.1-3%, lauric acid 0.1-2%, monoethanolamine 0.1-0.3%, hydrogenated castor oil 8-12%, pH adjuster 1-3%, water balance.

2. The method for preparing the hydrogenated castor oil suspension as described in claim 1, characterized in that, The preparation method includes the following steps: (1) Sodium linear alkylbenzene sulfonate and dodecanoic acid were added to some water, followed by monoethanolamine and pH adjuster to make the pH of the system 6-8. Then, sodium fatty alcohol polyoxyethylene ether sulfate was added and heated to 85-90℃. Hydrogenated castor oil was added to dissolve and homogenized to obtain O / W emulsion. (2) Add the remaining water to the O / W emulsion and homogenize it. Then cool it to 55-65℃ and keep it at that temperature for 0.5-1h. After the temperature is kept at that temperature, cool it to 50±2℃ at a cooling rate of 0.5-1.5℃ / min. Then turn off the homogenizer and turn on the stirring. Then cool it to below 40℃ to obtain hydrogenated castor oil suspension.

3. The application of the hydrogenated castor oil suspension as described in claim 1 or the hydrogenated castor oil suspension obtained by the preparation method as described in claim 2 in the preparation of microcapsule flavor beads.

4. A microcapsule flavoring bead, characterized in that, The microcapsule fragrance beads comprise a core and a coating layer, the core comprising a bead composition comprising the following components by weight percentage: The hydrogenated castor oil suspension as described in claim 1 or the hydrogenated castor oil suspension obtained by the preparation method described in claim 2 contains 8-16% anionic surfactant, 20-28% nonionic surfactant, 10-16% microencapsulated flavoring, 0.1-5% polymer, 3.5-6% monoethanolamine, 0-1% functional additives, and the balance being C3-C6 polyhydroxy alcohols; The anionic surfactant includes sulfonate anionic surfactants; The nonionic surfactant includes isomeric fatty alcohol alkoxylates; The C3-C6 polyhydroxy alcohols include propylene glycol and glycerol; The polymer includes a cationic acrylamide polymer.

5. The microcapsule flavor beads according to claim 4, characterized in that, The anionic surfactant also includes at least one of fatty acid salts, fatty alcohol polyether sulfates, and modified oil ethoxylate sodium sulfonate; And / or, the nonionic surfactant further includes at least one of fatty alcohol alkoxylates, fatty acid ester ethoxylates, oil ethoxylates, and fatty alcohol amide ethoxylates; And / or, the C3-C6 polyhydroxy group further includes at least one of isopropanol, 1,3-butanediol, erythritol, xylitol, sorbitol, and isohexyldiol; And / or, the polymer further includes polyethyleneimine ethoxylate; And / or, the functional additives include at least one of pigments, opacifiers, and bioenzymes.

6. The microcapsule flavor beads according to claim 5, characterized in that, The sulfonate anionic surfactant comprises 65-90% by mass, based on the mass of the anionic surfactant. And / or, based on the mass of the nonionic surfactant, the mass percentage of the isomeric fatty alcohol alkoxylate is 10-50%; And / or, based on the mass of the polymer, the cationic acrylamide polymer is 9-46% by mass; And / or, based on the total mass of the microcapsule flavor beads composition, the propylene glycol comprises 5-18% by mass and the glycerin comprises 15-30% by mass.

7. The microcapsule flavor beads according to claim 4, characterized in that, The sulfonate anionic surfactant includes at least one of linear alkylbenzene sulfonates and alkyl sulfonates; And / or, the isomeric fatty alcohol alkoxylates include at least one of isomeric AEO 7, products of the polymerization of isomeric C9-C11 alcohols with ethylene oxide, and products of the polymerization of isomeric C9-C11 alcohols with a mixture of ethylene oxide and propylene oxide.

8. The microcapsule flavor beads according to claim 4, characterized in that, The coating layer includes a water-soluble film, which includes any one of polyvinyl alcohol film, starch film, gelatin film, and polyvinyl acid film.

9. The method for preparing microcapsule flavor beads according to any one of claims 4-8, characterized in that, The preparation method includes the following steps: (1) A portion of C3-C6 polyhydroxy alcohols were mixed with hydrogenated castor oil suspending agent to obtain premix A; (2) Mix another portion of C3-C6 polyhydroxy alcohol with anionic surfactant and nonionic surfactant to obtain premix B; (3) Mix the remaining C3-C6 polyhydroxy alcohol with the microcapsule flavoring to obtain premix C; (4) After adjusting the pH of premix B to 7.5-8.5 and the temperature to 20-45℃, add premix A and stir for the first time, then add premix C and stir for the second time, then stir for the third time and add polymer and functional additives in sequence to obtain microcapsule flavor beads composition. (5) After vacuuming the microcapsule flavor gel beads composition, it is coated with a coating layer to obtain microcapsule flavor gel beads.

10. The preparation method according to claim 9, characterized in that, In step (1), the mass ratio of a portion of the C3-C6 polyhydroxy alcohol to the hydrogenated castor oil suspending agent is greater than or equal to 1. And / or, in step (3), the mass ratio of the remaining C3-C6 polyhydroxy alcohol to the microcapsule flavor is greater than or equal to 1.

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