Softener microcapsule, preparation method and application thereof

Abstract

The present invention relates to the technical field of softeners, and in particular to a softener microcapsule, a preparation method and application thereof. The softener microcapsule comprises a core layer and a shell layer; the core layer comprises silicone oil; the shell layer comprises plant protein and a non-cationic component, and the non-cationic component is melamine or melamine resin. The softener microcapsule of the present invention has good clothing adhesion and a certain strength, and is broken in time to release the softener when the clothing is rubbed.

Description

Technical Field

[0001] The present invention relates to the technical field of softeners, and in particular to a softener microcapsule, a preparation method and application thereof. Background Art

[0002] The main ingredients of existing softeners include cationic surfactants, lubricants and antistatic agents. Among them, the cationic surfactants of softeners are easily dispersed in water, have low adhesion to clothes, and are easily lost with water when washing and draining. In addition, some components of softeners need to rely on other types of surfactants to be dispersed in water, but the presence of surfactants will lead to a worse soft feel.

[0003] It can be seen that the existing technology still needs to be improved and enhanced. Summary of the invention

[0004] In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a softener microcapsule, a preparation method and application thereof, aiming to improve the adhesion and softening effect of the softener on clothes.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The first aspect of the present invention provides a softener microcapsule, comprising a core layer and a shell layer; the shell layer comprises plant protein and a non-cationic component, and the non-cationic component is melamine or melamine resin.

[0007] The softener microcapsule, wherein the thickness of the shell layer is 2 to 3 microns.

[0008] The softener microcapsules have a particle size of 18 to 22 microns.

[0009] The softener microcapsule, wherein the silicone oil includes polyether-modified silicone oil and amino-modified silicone oil.

[0010] The softener microcapsule, wherein the amino value of the amino-modified silicone oil is 50-200 mgKOH / g.

[0011] The softener microcapsule, wherein the mass ratio of the polyether-modified silicone oil to the amino-modified silicone oil is (2-5):1.

[0012] The second aspect of the present invention provides a method for preparing microcapsules, which is used to prepare the softener microcapsules as described above, comprising the following steps: adding silicone oil and shell layer raw materials into water, stirring and mixing at high speed at 50°C to obtain softener microcapsules.

[0013] The preparation method of the microcapsules, wherein the mass ratio of the silicone oil to the shell raw material is (31-37):(20-30); in the shell raw material, the mass ratio of the non-cationic component to the plant protein is 1:(3-7).

[0014] The preparation method of the microcapsules, wherein the mass ratio of the silicone oil to the shell raw material is (33-35):(25-28); in the shell raw material, the mass ratio of the non-cationic component to the plant protein is 1:(4-5).

[0015] The third aspect of the present invention provides the use of the softener microcapsules described above in fragrance beads, softeners, laundry tablets or laundry liquids.

[0016] Beneficial effects: The present invention provides a softener microcapsule, which has silicone oil as a core layer and plant protein and melamine or melamine resin as a shell layer, has good clothing adhesion, low loss rate during washing, and can release the silicone oil therein after being subjected to a certain pressure and friction, thereby playing a good lubricating effect. DETAILED DESCRIPTION

[0017] The present invention provides a softener microcapsule, a preparation method and application thereof. To make the purpose, technical solution and effect of the present invention clearer and more specific, the present invention is further described in detail with reference to the following examples. It should be understood that the specific examples described herein are only used to explain the present invention and are not used to limit the present invention.

[0018] The first aspect of the present invention provides a softener microcapsule, comprising a core layer and a shell layer; the shell layer comprises plant protein and a non-cationic component, and the non-cationic component is melamine or melamine resin.

[0019] In the present invention, silicone oil is the main component that plays a softening role. It can form a thin film covering the surface of clothing, making the clothing soft, smooth, easy to iron, and reducing the generation of static electricity. Melamine and melamine resin can form microcapsules in water, thereby coating silicone oil to form a shell layer. Compared with the prior art, silicone oil, melamine or melamine resin are not surfactants, which can avoid causing the soft feel to deteriorate. In addition, melamine or melamine resin has good adhesion to clothes, and can reduce the loss of softener with water when using softener. In addition, the microcapsule structure formed by coating silicone oil with melamine or melamine resin has good structural strength in water, is not easy to break during washing, and can effectively reduce the loss of silicone oil in water. Plant protein such as bean protein has gel and emulsification properties in the microencapsulation delivery system, which can further improve the shell structure. Plant protein is amphiphilic, that is, it has both hydrophilicity and hydrophobicity. The hydrophobic end of the plant protein is connected to the silicone oil, and the hydrophilic end is located on the outside of the shell layer. From the outside, plant protein has good adhesion to clothing. With the good adhesion of plant protein, melamine or melamine resin to clothing, more microcapsules can be retained on the clothes. After drying, the microcapsules can be easily broken by friction, releasing silicone oil, which has a softening effect.

[0020] Preferably, the thickness of the shell layer is 1 to 10 microns. The thickness of the shell layer should not be too small, otherwise it is easy to break and the silicone oil is easy to lose. The thickness of the shell layer should not be too large, otherwise it is difficult for the shell layer to pass through friction and the silicone oil cannot be released at the appropriate time.

[0021] Preferably, the thickness of the shell layer is 2 to 3 microns. Within this thickness range, the shell layer has the best strength, which can meet the strength requirements of the early washing process and the later release process.

[0022] Preferably, the particle size of the softener microcapsule is 18 to 22 microns. The overall particle size of the softener microcapsule will also affect the structural strength of the microcapsule. When the thickness of the shell layer remains unchanged, the larger the particle size of the softener microcapsule, the larger the volume of the core layer, and the greater the internal pressure formed, which makes the microcapsule easier to rupture. If the particle size is too small, the silicone oil contained is correspondingly less, and the lubricating effect is limited. At the same time, if the particle size of the microcapsule is too small, it is also more difficult to rupture, which is not conducive to the release of silicone oil.

[0023] Preferably, the silicone oil includes polyether-modified silicone oil and amino-modified silicone oil. Amino-modified silicone oil has good adsorption, compatibility and easy emulsification. By compounding polyether-modified silicone oil and amino-modified silicone oil, the softening effect can be better.

[0024] Preferably, the amino modified silicone oil has an ammonia value of 50 to 200 mgKOH / g. The higher the ammonia value, the better the softness and slipperiness, but the yellowing will increase.

[0025] Preferably, the mass ratio of the polyether-modified silicone oil to the amino-modified silicone oil is (2-5): 1. Within the above ratio range, the softening effect of the composite system is the best.

[0026] Preferably, the plant protein includes at least one of soy protein, chickpea protein, pea protein and barley protein.

[0027] The second aspect of the present invention provides a method for preparing microcapsules, which is used to prepare the softener microcapsules as described above, comprising the following steps: adding silicone oil, plant protein and non-cationic components into water, stirring and mixing at high speed at 50°C to obtain softener microcapsules.

[0028] Preferably, the mass ratio of the silicone oil to the shell raw material is (31-37):(20-30); in the shell raw material, the mass ratio of the non-cationic component to the plant protein is 1:(3-7).

[0029] In a further preferred embodiment, the mass ratio of the silicone oil to the shell material is (33-35):(25-28); in the shell material, the mass ratio of the non-cationic component to the plant protein is 1:(4-5). Within the above mass ratio range, the particle size of the softener microcapsules formed is in the optimal range, and the shell thickness is also in the optimal range.

[0030] The third aspect of the present invention provides the use of the softener microcapsules described above in fragrance beads, softeners, laundry tablets or laundry liquids.

[0031] Example 1

[0032] A softener microcapsule, the preparation method of which comprises the following steps:

[0033] 350 parts of silicone oil, 50 parts of melamine and 200 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0034] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0035] Example 2

[0036] A softener microcapsule, the preparation method of which comprises the following steps:

[0037] 310 parts of silicone oil, 25 parts of melamine and 175 parts of pea protein were added to 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0038] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0039] Example 3

[0040] A softener microcapsule, the preparation method of which comprises the following steps:

[0041] 370 parts of silicone oil, 75 parts of melamine and 225 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0042] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0043] Example 4

[0044] A softener microcapsule, the preparation method of which is different from that of Example 1 in that the silicone oil consists of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 2:1.

[0045] Example 5

[0046] A softener microcapsule, the preparation method of which is different from that of Example 1 in that the silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 5:1.

[0047] Example 6

[0048] A softener microcapsule, the preparation method of which comprises the following steps:

[0049] 330 parts of silicone oil, 50 parts of melamine resin and 230 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0050] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0051] Example 7

[0052] A softener microcapsule, the preparation method of which comprises the following steps:

[0053] 340 parts of silicone oil, 40 parts of melamine resin and 240 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50° C. to prepare softener microcapsules;

[0054] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0055] Example 8

[0056] A softener microcapsule, the preparation method of which comprises the following steps:

[0057] 350 parts of silicone oil, 50 parts of melamine, and 200 parts of pea protein were added to 600 parts of water, and stirred at high speed (10000r / min) for 10 minutes at 50°C to obtain softener microcapsules.

[0058] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 6:1; the ammonia value of the amino-modified silicone oil is 50 mgKOH / g.

[0059] Example 9

[0060] A softener microcapsule, the preparation method of which comprises the following steps:

[0061] 350 parts of silicone oil, 50 parts of melamine and 200 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0062] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 1:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0063] Example 10

[0064] A softener microcapsule, the preparation method of which comprises the following steps:

[0065] 350 parts of silicone oil, 50 parts of melamine and 200 parts of pea protein were added into 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0066] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 6:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0067] Comparative Example 1

[0068] A softener microcapsule, the preparation method of which comprises the following steps:

[0069] 300 parts of silicone oil, 75 parts of melamine and 225 parts of pea protein were added to 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50° C. to prepare softener microcapsules;

[0070] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0071] Comparative Example 2

[0072] A softener microcapsule, the preparation method of which comprises the following steps:

[0073] 370 parts of silicone oil, 50 parts of melamine and 150 parts of pea protein were added to 600 parts of water, and stirred at high speed (10000 r / min) for 10 minutes at 50°C to prepare softener microcapsules;

[0074] The silicone oil is composed of polyether-modified silicone oil and amino-modified silicone oil in a mass ratio of 3:1; the ammonia value of the amino-modified silicone oil is 160 mgKOH / g.

[0075] 1. Use a microscope to measure the particle size of the above softener microcapsules.

[0076] 2. The strength of the microcapsules was characterized by an indirect determination method by measuring the amount of content released from the softener microcapsules. The method is as follows: Based on the preparation methods of the above embodiments and comparative examples, a low-boiling point flavor (boiling point of 75-78°C) was added to the silicone oil, and the mass ratio of silicone oil to flavor was 99:1, and then the softener microcapsules were further prepared. The content M of the flavor was measured by headspace injection. Headspace injection conditions: heating box temperature: 60°C, quantitative loop temperature: 65°C, transmission line: 105°C, sample equilibration time: 30min, GC cycle: 45min. Silicone oil content A1 = (M ÷ 1) × 99, breakage rate = silicone oil content A1 ÷ silicone oil content A2 in microcapsules × 100%.

[0077] 3. Determine the softening effect of the softener microcapsules. The softening effect test is carried out in accordance with GB / T18318.1-2009 and is expressed by the reduction value of the straight bending length ΔL. Wherein, ΔL: the change in bending length before and after fabric treatment, accurate to one decimal place; L before treatment: the bending length of fabric before treatment, in cm; L after treatment: the bending length of fabric after treatment, in cm; Note: the smaller the straight bending length, the better the softening effect of the laundry composition. The pretreatment method is: the laundry composition is fully dissolved in deionized water, and the fabric sample to be tested is put into the bath ratio of 1:50, stirred and soaked for 20 minutes (stirred once every 5 minutes, each time for 30 seconds), taken out and dehydrated, and dried at 80℃ for use.

[0078] 4. Determine the effect of softener microcapsules on the attachment of clothes as follows: add three pieces of laundry to a softener microcapsule solution of a specific concentration and soak for 50 minutes. Then observe the residual amount of softener microcapsule solution in the dehydration liquid under a microscope, and calculate the attachment rate based on the number of microcapsules per unit volume in the solution before washing and the number of microcapsules per unit volume in the solution after washing.

[0079] The particle size distribution and shell thickness of the microcapsules of the above embodiments and comparative examples are shown in Table 1, and the microcapsule breakage rate, bending length reduction value and microcapsule attachment rate are shown in Table 2.

[0080] Table 1

[0081] Particle size (micrometers) Example 1 20 Example 2 25 Example 3 19 Example 4 22 Example 5 22 Example 6 18 Example 7 18 Example 8 21.5 Example 9 22.5 Example 10 21.8 Comparative Example 1 14 Comparative Example 2 29

[0082] Table 2

[0083]

[0084]

[0085] From the above results, it can be seen that the particle sizes of the softener microcapsules of Examples 1-10 are all between 18 and 25, the breakage rates are all below 46%, and the lowest can reach 24%, with good strength, good softening effect, and high adhesion rate.

[0086] Compared with Examples 1-10, Comparative Example 1 uses less silicone oil and more shell material, and the microcapsule wall strength is higher. Although its breakage rate is low, the microcapsules are not easy to break, the silicone oil is not easy to release, and the softening effect is also limited.

[0087] Compared with Examples 1-10, Comparative Example 2 uses more silicone oil and less shell material, and the strength of the microcapsule wall formed is relatively low, which leads to a high breakage rate, a large loss of silicone oil, and a reduced softening effect.

[0088] Further comparison of Example 1, Examples 4-5, and Examples 9-10 revealed that when the mass ratio of the polyether-modified silicone oil to the amino-modified silicone oil was (2-5):1, the softening effect was best.

[0089] It is understandable that those skilled in the art can make equivalent substitutions or changes based on the technical solution and inventive concept of the present invention, and all these changes or substitutions should fall within the protection scope of the claims attached to the present invention.

Claims

1. A softener microcapsule, characterized in that: It comprises a core layer and a shell layer; the core layer comprises silicone oil; the shell layer comprises vegetable protein and non-cationic components, and the non-cationic components are melamine or melamine resin.

2. The softener microcapsule according to claim 1, characterized in that: The thickness of the shell layer is 2 to 3 microns.

3. The softener microcapsule according to claim 2, characterized in that: Its particle size is 18 to 22 microns.

4. The softener microcapsule according to claim 1, characterized in that: The silicone oil includes polyether-modified silicone oil and amino-modified silicone oil; the ammonia value of the amino-modified silicone oil is 50-200 mgKOH / g.

5. The softener microcapsule according to claim 4, characterized in that: The mass ratio of the polyether modified silicone oil to the amino modified silicone oil is (2-5):

1.

6. The softener microcapsule according to claim 1, characterized in that: The plant protein comprises at least one of soy protein, chickpea protein, pea protein and barley protein.

7. A method for preparing microcapsules, characterized in that: The method for preparing the softener microcapsules as claimed in any one of claims 1 to 6 comprises the following steps: adding silicone oil and shell layer raw materials into water, stirring and mixing at high speed at 50° C. to obtain softener microcapsules.

8. The method for preparing microcapsules according to claim 7, characterized in that: The mass ratio of the silicone oil to the shell raw material is (31-37):(20-30); in the shell raw material, the mass ratio of the non-cationic component to the plant protein is 1:(3-7).

9. The method for preparing microcapsules according to claim 8, characterized in that: The mass ratio of the silicone oil to the shell raw material is (33-35):(25-28); in the shell raw material, the mass ratio of the non-cationic component to the plant protein is 1:(4-5).

10. Use of the softener microcapsule according to any one of claims 1 to 6 in fragrance beads, softener, laundry tablets or laundry liquid.

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