Organic silicon softener material for towels, preparation method and application thereof

Abstract

The present application discloses a kind of organic silicon softener material, preparation method and application for towels, wherein the preparation method of organic silicon softener material for towels comprises the following steps, S1: reacting 2-aminoimidazole and polyethylene glycol diglycidyl ether in an organic solvent to obtain polyether-modified imidazole; S2: catalyzing reaction of side hydrogen-containing silicone oil and allyl polyoxyethylene ether glycidyl ether to obtain polyether-modified silicone oil; S3: reacting polyether-modified imidazole, polyether-modified silicone oil and disodium glutamate aqueous solution, and obtaining organic silicon softener material for towels after removing impurities. The organic silicon softener of the present application has good stability, and gives the towels good feel, softness, antibacterial effect and water absorption after treating the towels.

Description

Technical Field

[0001] The present application relates to the field of polymer materials, and in particular to an organosilicon softener material for towels, a preparation method and application thereof. Background Art

[0002] Towels are one of the fabrics that come into direct contact with the human body, so people have very high requirements for their comfort. They are not only required to have excellent hydrophilic properties and high water holding rate, but also to have a fluffy and soft feel. Silicone softeners play an important role in textiles such as towels, which can improve the softness and smoothness of towels and improve their durability. Silicone softeners can not only improve the quality and added value of products, but also have the characteristics of being environmentally friendly and human-friendly.

[0003] The softening process of towels is usually softened by soaking in a vat, which has high requirements for product stability. As the environmental protection pressure of printing and dyeing enterprises is increasing and the cost control is becoming more and more stringent, many enterprises will choose to use recycled treated water or choose a process with less water for softening. At this time, the recycled treated water contains more metal ion impurities. If the recycled treated water is mixed with silicone softener, it is likely to cause demulsification and oil floating of the finishing working fluid, which may cause oil spots and defects on the cloth.

[0004] In addition, most of the commercially available silicone softeners for towels are highly cationic softeners, and it is difficult to achieve both electrolyte resistance stability and comfort performance. Therefore, the market urgently needs to develop silicone finishing agents with excellent performance, electrolyte resistance stability and low charge. Summary of the invention

[0005] The purpose of this application is to improve the stability of the organosilicon softener for towels.

[0006] Another object of the present application is to improve the performance of silicone softeners for towels.

[0007] In order to achieve the above purpose, the technical solution adopted in this application is: to provide a silicone softener material for towels, the general structural formula of which is:

[0008]

[0009] Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

[0010] The present application also provides a method for preparing a silicone softener material for towels, comprising the following preparation steps:

[0011] S1: 2-aminoimidazole and polyethylene glycol diglycidyl ether react in an organic solvent to obtain polyether-modified imidazole; S2: side hydrogen-containing silicone oil and allyl polyoxyethylene ether glycidyl ether are catalyzed to obtain polyether-modified silicone oil; S3: the polyether-modified imidazole, the polyether-modified silicone oil and a disodium glutamate aqueous solution are reacted to obtain the organic silicone softener material for towels after impurities are removed;

[0012] The general structural formula of the polyether-modified imidazole is:

[0013]

[0014] Where n is an integer, and 1≤n≤6;

[0015] The general structural formula of the polyether modified silicone oil is:

[0016]

[0017] Wherein a, c, d, e, m are integers, and 0≤a≤263, 0≤c≤263, 1≤d≤5, 4≤e≤10, 9≤m≤20;

[0018] The general structural formula of the organosilicon softener material for towels is:

[0019]

[0020] Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

[0021] As a preference, the number average molecular weight of the polyethylene glycol diglycidyl ether is 200-400.

[0022] As a preference, the number average molecular weight of the side hydrogen-containing silicone oil is 20,000-30,000, and the hydrogen content of the side hydrogen-containing silicone oil is 0.027%-0.05%.

[0023] As a preference, the number average molecular weight of the allyl polyoxyethylene ether glycidyl ether is 500-1000.

[0024] As a preferred embodiment, the S1 step is specifically as follows, by mass: 166 parts of the 2-aminoimidazole and 366 to 566 parts of the organic solvent are added to the reaction device, stirred and heated, and after the 2-aminoimidazole is completely dissolved, 200 to 400 parts of the polyethylene glycol diglycidyl ether are slowly added to the reaction device, and the polyether-modified imidazole is obtained after keeping warm for 4 to 6 hours.

[0025] As a preferred embodiment, the S2 step is specifically as follows, calculated by mass: 2000-3000 parts of the side hydrogenated silicone oil and 200-1000 parts of the allyl polyoxyethylene ether glycidyl ether are reacted in a reaction device, and then 940-1715 parts of an organic solvent and 2-3 parts of a catalyst are added to the reaction device, and the temperature is increased and kept warm for 6-8 hours to obtain the polyether-modified silicone oil.

[0026] As a preferred embodiment, the S3 step is specifically as follows, by mass: 3140 to 5715 parts of the polyether-modified silicone oil, 146 to 566 parts of the polyether-modified imidazole and 76 to 191 parts of the disodium glutamate aqueous solution are added to the reaction device, and then 1256 to 2285 parts of the organic solvent are added, the temperature is increased and kept for a period of time, and finally the impurities in the product are removed.

[0027] As another preference, the mass fraction of disodium glutamate in the disodium glutamate aqueous solution is 30% to 60%.

[0028] The present application also provides a silicone softener for towels, which is made from the following raw materials in parts by mass: 200 to 300 parts of deionized water, 2 to 4 parts of glacial acetic acid, 15 to 30 parts of emulsifier, and 80 to 120 parts of the above-mentioned silicone softener material for towels, or the silicone softener material for towels prepared by the above-mentioned preparation method.

[0029] Compared with the prior art, the beneficial effects of this application are:

[0030] (1) The organic silicone softener material for towels of the present application introduces aminoimidazole groups into the structure to impart certain antibacterial properties to the material, so that the treated fabric has a good bacterial inhibition rate;

[0031] (2) The organic silicone softener material for towels of the present application has a structure designed to reduce the charge of the product through the synergistic effect of the carboxylate group and the amino group, thereby further reducing the lint loss of fabrics such as towels after treatment;

[0032] (3) The organic silicone softener material for towels of the present application has a synergistic effect of the carboxylic acid group and the polyether segment in the structure, and the product can maintain stable properties in more complex environments;

[0033] (4) The organic silicon softener material for towels of the present application has an amino group, an imidazole group, a polyether segment and an organic silicon segment in its structure that work together to give the treated towel fabric excellent practicality. DETAILED DESCRIPTION

[0034] Below, the present application is further described in conjunction with specific implementation methods. It should be noted that, under the premise of no conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0035] The terms "including" and "having" and any variations thereof in the specification and claims of this application are intended to cover non-exclusive inclusions. For example, a process, method, system, product or apparatus comprising a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to these processes, methods, products or apparatuses.

[0036] The present application provides a silicone softener material for towels, the general structural formula of which is as follows:

[0037]

[0038] Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

[0039] The organosilicon softener for towels of the present application has an aminoimidazole structure designed in its structure, which can inhibit the formation of biofilm, thereby destroying the self-protection ability of bacteria. It is used in the post-processing of towels, fabrics and other products and has a certain antibacterial effect.

[0040] The organic silicon softener for towels of the present application has a carboxylate group in its structure, which works synergistically with the amino group to reduce the charge of the product and reduce the linting phenomenon of the towels during the softening process. In addition, the carboxylate group and the polyether chain segment synergistically improve the stability of the product, so that the organic silicon finishing agent can be used in more complex environments.

[0041] The organosilicon softener for towels of the present application has a structure in which the amino group, imidazole structure, polyether and organosilicon segment structure work synergistically to give the product fluffy and soft performance and excellent water holding capacity.

[0042] The present application provides a method for preparing an organosilicon softener material for towels, comprising the following preparation steps, wherein the raw materials in the steps are calculated by weight:

[0043] S1: 2-aminoimidazole and polyethylene glycol diglycidyl ether are reacted in a solvent to prepare a polyether-modified imidazole;

[0044] S2: preparing polyether modified silicone oil by catalytic reaction of side hydrogen-containing silicone oil and allyl polyoxyethylene glycidyl ether;

[0045] S3: polyether-modified imidazole, polyether-modified silicone oil and disodium glutamate aqueous solution are reacted, and after removing impurities, an organosilicon softener material for towels is obtained.

[0046] In step S1, 2-aminoimidazole and polyethylene glycol diglycidyl ether are reacted to obtain polyether-modified imidazole according to the following reaction formula:

[0047]

[0048] Wherein n is an integer, and 1≤n≤6.

[0049] In step S2, the reaction formula for preparing polyether-modified silicone oil from hydrogenated silicone oil and allyl polyoxyethylene glycidyl ether is as follows:

[0050]

[0051] Wherein a, b, c, d, e, m are integers and 0≤a≤263, 5≤b≤15, 0≤c≤263, 1≤d≤5, 4≤e≤10, 9≤m≤20.

[0052] In step S3, the reaction formula for generating the organic silicone softener material for towels from polyether-modified imidazole, polyether-modified silicone oil and disodium glutamate aqueous solution is as follows:

[0053]

[0054] Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 4≤e≤10, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

[0055] The present application utilizes the epoxy curing mechanism and uses a double-ended epoxy polyether to modify 2-aminoimidazole to obtain a polyether-modified imidazole, and then utilizes the obtained polyether-modified imidazole and the secondary amine and primary amine in the amino acid salt to react with the epoxy group of epoxy silicone oil to obtain a silicone softener material for towels, which is suitable for the post-processing process of fabrics such as towels.

[0056] In some embodiments, step S1 is specifically as follows: 166 parts by mass of 2-aminoimidazole and 366 to 566 parts by mass of an organic solvent are added to a reaction device, stirred and heated, and after the 2-aminoimidazole is completely dissolved, 200 to 400 parts by mass of polyethylene glycol diglycidyl ether are slowly added to the reaction device, and the product polyether-modified imidazole is obtained after keeping warm for 4 to 6 hours.

[0057] In some preferred embodiments, the number average molecular weight of polyethylene glycol diglycidyl ether is 200-400.

[0058] In some embodiments, step S2 is specifically as follows: reacting 2000-3000 parts by mass of hydrogenated silicone oil and 200-1000 parts by mass of allyl polyoxyethylene ether glycidyl ether in a reaction device, adding 940-1715 parts by mass of an organic solvent and 2-3 parts by mass of a catalyst to the reaction device, heating and keeping the reaction for 6-8 hours to obtain a polyether-modified silicone oil.

[0059] In some preferred embodiments, the number average molecular weight of the hydrogen-containing silicone oil is 20,000-30,000.

[0060] In some preferred embodiments, the hydrogen content of the hydrogen-containing silicone oil is 0.027% to 0.05%.

[0061] In some preferred embodiments, the number average molecular weight of allyl polyoxyethylene ether glycidyl ether is 500-1000.

[0062] In some preferred embodiments, the catalyst is a 2% chloroplatinic acid-isopropanol solution.

[0063] In some embodiments, step S3 is specifically as follows: 3140 to 5715 parts by mass of polyether-modified silicone oil, 146 to 566 parts by mass of polyether-modified imidazole and 76 to 191 parts by mass of disodium glutamate aqueous solution are added to a reaction device, and then 1256 to 2285 parts by mass of an organic solvent are added, the temperature is increased and kept warm for a period of time, and finally the impurities in the product are removed to obtain the silicone softener material for towels of the present application.

[0064] In some embodiments, the mass fraction of disodium glutamate in the disodium glutamate aqueous solution is 30% to 60%, preferably 50%.

[0065] In some embodiments, the synthesized product is subjected to organic solvent removal under vacuum negative pressure of -0.09 to -0.1 MPa, and after removing 1900 to 3605 parts by mass of organic solvent, the organosilicon softener material for towels of the present application is obtained.

[0066] In some embodiments, the organic solvent used in step S1, step S2, and step S3 is isopropanol.

[0067] The reaction process of the preparation process of the organosilicon softener material for towels of the present application is easy to control and suitable for industrial production.

[0068] A preferred solution of this application is:

[0069] S1: 166 parts by mass of 2-aminoimidazole and 366 parts by mass of isopropanol are added to a reaction kettle equipped with a thermometer, a stirrer, and a condensation reflux, stirring is started, and the temperature is raised to 40° C. After the 2-aminoimidazole is completely dissolved, 200 parts by mass of polyethylene glycol diglycidyl ether with a number average molecular weight of 200 is slowly added dropwise to the reaction kettle, and the temperature is kept for 4 hours to obtain a polyether-modified imidazole;

[0070] S2: 3000 parts by mass of a side hydrogenated silicone oil with a number average molecular weight of 30000 and a hydrogen content of 0.05% and 1000 parts by mass of allyl polyoxyethylene ether glycidyl ether with a number average molecular weight of 1000 are added to a reaction kettle equipped with a thermometer, a stirrer, and a condensation reflux, 1715 parts by mass of isopropanol and 3 parts by mass of a 2% chloroplatinic acid-isopropanol solution are added, the temperature is raised to 75° C., and the temperature is kept for 6 hours to obtain a polyether-modified silicone oil;

[0071] S3: 5715 parts by mass of polyether-modified silicone oil, 336 parts by mass of polyether-modified imidazole and 191 parts by mass of 50% disodium glutamate aqueous solution are added to a reactor equipped with a thermometer, a stirrer and a condensation reflux, and 2285 parts by mass of isopropanol are added. The temperature is raised to 75°C. After keeping warm for 12 hours, 3510 parts by mass of isopropanol are removed under a vacuum negative pressure of -0.09 MPa to obtain the silicone softener material for the towels of the present application.

[0072] The present application provides an organic silicone softener for towels, comprising the following raw materials in parts by weight: 200 to 300 parts of deionized water, 2 to 4 parts of glacial acetic acid, 15 to 30 parts of emulsifier, and 80 to 120 parts of the organic silicone softener material for towels of the present application.

[0073] The organic silicon softener for towels of the present application can stably exist in an anionic or electrolyte environment, is suitable for more application environments, and has good hand feel, softness, water absorption and certain antibacterial effect.

[0074] Example 1

[0075] A silicone softener for towels is prepared according to the following preparation steps, wherein the amount of each raw material added is calculated by weight:

[0076] S1: 166 parts of 2-aminoimidazole and 366 parts of isopropanol are added to a reaction kettle equipped with a thermometer, a stirrer, and a condensation reflux, stirring is started, and the temperature is raised to 40°C. After the 2-aminoimidazole is completely dissolved, 200 parts of polyethylene glycol diglycidyl ether with a number average molecular weight of 200 are slowly added dropwise to the reaction kettle, and the temperature is kept for 4 hours to obtain a polyether-modified imidazole;

[0077] S2: 2000 parts of side hydrogen-containing silicone oil with a number average molecular weight of 20000 and a hydrogen content of 0.027% and 200 parts of allyl polyoxyethylene ether glycidyl ether with a number average molecular weight of 500 are added to a reaction kettle equipped with a thermometer, a stirrer, and a condensation reflux, 940 parts of isopropanol and 2 parts of a 2% chloroplatinic acid-isopropanol solution are added, the temperature is raised to 75° C., and the temperature is kept for 6 hours to obtain a polyether-modified silicone oil;

[0078] S3: 3140 parts of polyether-modified silicone oil, 146 parts of polyether-modified imidazole and 76 parts of 50% disodium glutamate aqueous solution are added to a reaction kettle equipped with a thermometer, a stirrer and a condensation reflux, and 1256 parts of isopropanol are added. The temperature is raised to 75° C. After keeping warm for 12 hours, 1900 parts of isopropanol are removed under a vacuum negative pressure of -0.09 MPa to obtain the silicone softener material for towels of the present application.

[0079] Preparation of silicone softener for towels: 100 parts by mass of silicone softener material for towels, 20 parts by mass of emulsifier 1350, 240 parts by mass of deionized water and 2 parts by mass of glacial acetic acid are added into a high shear homogenization emulsification kettle, and the silicone softener for towels is emulsified.

[0080] Example 2

[0081] In step S1, polyethylene glycol diglycidyl ether with a number average molecular weight of 400 is selected, and its addition amount is adjusted to 400 parts by mass;

[0082] The amount of polyether-modified imidazole added in step S3 is adjusted to 226 parts by mass, the amount of disodium glutamate aqueous solution added is adjusted to 38 parts by mass, and 1920 parts by mass of isopropanol is removed under vacuum negative pressure conditions;

[0083] The other preparation steps are consistent with those in Example 1.

[0084] Example 3

[0085] In step S2, allyl polyoxyethylene glycidyl ether with a number average molecular weight of 1000 is selected and its addition amount is adjusted to 400 parts by mass, and the addition amount of isopropanol is correspondingly adjusted to 1028 parts by mass;

[0086] In step S3, the amount of polyether-modified silicone oil added is adjusted to 3428 parts by mass, the amount of isopropanol solvent added is adjusted to 1370 parts by mass, and finally 2070 parts by mass of isopropanol are removed under vacuum negative pressure conditions;

[0087] The other preparation steps are consistent with those in Example 1.

[0088] Example 4

[0089] In step S2, the hydrogen content of the side hydrogenated silicone oil is adjusted to 0.05%, the amount of allyl polyoxyethylene ether glycidyl ether is adjusted to 400 parts by mass, and the amount of isopropanol is adjusted to 1028 parts by mass to obtain a polyether-modified silicone oil;

[0090] In step S2, the amount of polyether-modified silicone oil added is adjusted to 3428 parts by mass, the amount of polyether-modified imidazole added is adjusted to 336 parts by mass, the amount of 50% disodium glutamate aqueous solution added is adjusted to 191 parts by mass, and the amount of isopropanol added is adjusted to 1370 parts by mass, and finally 2190 parts by mass of isopropanol are removed under vacuum conditions;

[0091] The other preparation steps are consistent with those in Example 1.

[0092] Example 5

[0093] In step S2, a side hydrogen-containing silicone oil with a number average molecular weight of 30,000 is selected and its addition amount is adjusted to 3,000 parts by mass, the addition amount of isopropanol is adjusted to 1,370 parts by mass, and the addition amount of 2% chloroplatinic acid-isopropanol solution is adjusted to 3 parts by mass;

[0094] In step S3, the amount of polyether-modified silicone oil added is adjusted to 4570 parts by mass, the amount of isopropanol solvent added is adjusted to 1828 parts by mass, and finally 2720 parts by mass of isopropanol are removed under vacuum negative pressure conditions;

[0095] The other preparation steps are consistent with those in Example 1.

[0096] Example 6

[0097] In step S2, the hydrogen content of the hydrogenated silicone oil is adjusted to 0.05%, the amount of allyl polyoxyethylene ether glycidyl ether is adjusted to 500 parts by mass, and the amount of isopropanol is adjusted to 1500 parts by mass;

[0098] In step S3, the amount of polyether-modified silicone oil added is adjusted to 5000 parts by mass, the amount of polyether-modified imidazole added is adjusted to 336 parts by mass, the amount of 50% disodium glutamate aqueous solution added is adjusted to 191 parts by mass, and the amount of isopropanol added is adjusted to 2000 parts by mass, and finally 3100 parts by mass of isopropanol are removed under vacuum negative pressure conditions;

[0099] The other preparation steps are consistent with those in Example 5.

[0100] Example 7

[0101] In step S2, allyl polyoxyethylene ether glycidyl ether with a number average molecular weight of 1000 is selected and its addition amount is adjusted to 1000 parts by mass, and the addition amount of isopropanol is adjusted to 1715 parts by mass;

[0102] In step S3, the amount of polyether-modified silicone oil added is adjusted to 5715 parts by mass, the amount of isopropanol added is adjusted to 2285 parts by mass, and finally 3510 parts by mass of isopropanol are removed under vacuum negative pressure conditions;

[0103] The other preparation steps are consistent with those in Example 6.

[0104] Example 8

[0105] In step S1, polyethylene glycol diglycidyl ether with a number average molecular weight of 400 is selected and its addition amount is adjusted to 400 parts by mass, and the addition amount of isopropanol is adjusted to 566 parts by mass;

[0106] In step S3, the amount of polyether-modified imidazole added was adjusted to 556 parts by mass, and finally 3190 parts by mass of isopropanol were removed under vacuum conditions;

[0107] The other preparation steps are consistent with those in Example 6.

[0108] Example 9

[0109] The insulation time in step S2 was adjusted to 8 hours, and the other preparation steps were consistent with the preparation steps in Example 7.

[0110] Example 10

[0111] The insulation time in step S2 was adjusted to 16 hours, and the other preparation steps were consistent with the preparation steps in Example 7.

[0112] Comparative Example 1

[0113] The polyether-modified imidazole in step S3 was replaced with a corresponding proportion of polyetheramine ED400, and the other preparation steps were consistent with those in Example 7.

[0114] Comparative Example 2

[0115] The 50% disodium glutamate aqueous solution in step S3 was replaced with propylenediamine in a corresponding proportion, and the other preparation steps were consistent with the preparation steps in Example 7.

[0116] Comparative Example 3

[0117] Purchase a commercially available silicone oil for towels.

[0118] Comparative Example 4

[0119] Purchase another commercially available silicone oil for towels.

[0120] Performance Testing

[0121] Anion resistance stability test: 6 g of the silicone softener emulsion prepared in each embodiment and each comparative example was added to 197 mL of sodium dodecyl sulfate solution, wherein the temperature was raised to 50° C., and the state of the emulsion in the beaker was observed after standing for 4 hours to check whether the emulsion showed demulsification, stratification, oil floating, etc., so as to judge the anion resistance stability of the silicone softener. The test results are recorded in Table 1 below.

[0122] Electrolyte resistance stability test: 6 g of the silicone softener emulsion prepared in each embodiment and each comparative example was added to a mixed solution prepared by dissolving 5 g / L of sodium sulfate and 15 g / L of sodium carbonate in water. The mixed solution was heated to 50° C. and allowed to stand for 4 h. Whether demulsification, stratification, and floating oil appeared in the beaker was observed to determine the electrolyte resistance stability of the silicone softener. The test results were recorded in Table 1 below.

[0123] Table 1 Stability test results of silicone softener

[0124] Anion stability Electrolyte resistance and stability Example 1 Stablize Stablize Example 2 Stablize Stablize Example 3 Stablize Stablize Example 4 Stablize Stablize Example 5 Stablize Stablize Example 6 Stablize Stablize Example 7 Stablize Stablize Example 8 Stablize Stablize Example 9 Stablize Stablize Example 10 Stablize Stablize Comparative Example 1 Stablize Stablize Comparative Example 2 Demulsification and oil bleaching Demulsification and oil bleaching Comparative Example 3 Demulsification and oil bleaching Demulsification and oil bleaching Comparative Example 4 Demulsification and oil bleaching Demulsification and oil bleaching

[0125] It is not difficult to see from the results of the silicone softener stability test in Table 1 that the silicone softeners prepared in Comparative Examples 2, 3 and 4 cannot stably exist in an anionic environment or an electrolyte environment, and demulsification and oil floating phenomena occur. In the preparation process of Comparative Example 2, propylene diamine is used to replace disodium glutamate, so that the structure of the silicone softener prepared in Comparative Example 2 does not contain a carboxylic acid structure, which indicates that the carboxylic acid structure contained in the silicone softener of the present application can synergize with the polyether segment, and has the effect of improving the stability of the silicone softener product, so that the silicone softener has more application scenarios, and it will not destroy the structure of the silicone softener when mixed with the circulating treated water in the process of soaking and softening towels.

[0126] However, the two commercially available silicone oils for towels cannot exist stably in anionic and electrolyte environments. Their application environment is relatively limited. During the towel processing process, they are affected by other processes, causing the softener to become ineffective and the towel's usability to decline.

[0127] Evaluation of the application performance of cotton towel fabric: The cotton towel fabric was impregnated with a silicone softener working solution containing 15 g / L of silicone softener. After soaking the towel for 15 minutes, it was placed in an oven and dried at 120°C for 8 to 12 minutes. After regaining moisture for 1 hour, the hand feel evaluation test, softness test, antibacterial performance test and water absorption test were performed. The test results are recorded in Table 2 below.

[0128] Hand feel evaluation test: Use hand touch method to evaluate the comprehensive hand feel, using a 1-5 point evaluation method, 1 point is the worst and 5 points is the best. 10 people evaluate at the same time and take the average value.

[0129] Softness: According to GB / T18318 "Textiles·Determination of Bending Length of Fabrics": Take a long strip sample and place it on the platform, press a ruler on the sample, and the long axis of the sample is parallel to the length direction of the ruler. The ruler and the long axis direction of the sample move on the platform at the same time, so that the sample protrudes from the platform and is suspended in the air, and bends under its own weight. When the downward bent end of the sample touches the inclined plane at an angle of 41.5° to the horizontal, 1 / 2 of the protruding length of the sample is the bending length. The bending stiffness of the sample is calculated by the bending length and the mass per unit area. Sample: 6 pieces of 25mm*25mm warp and weft knitting, each sample is measured 4 times, and the average value is taken;

[0130] Calculation of flexural stiffness:

[0131] G=mC 3 10 -2

[0132] Where: G——bending stiffness per unit width, mN·cm;

[0133] m——mass per unit area of ​​the sample, g / m 2 ;

[0134] C is the average bending length of the specimen, cm.

[0135] Evaluation of antibacterial performance: Test according to the "Test Method for Antibacterial Performance of Fabrics (FZ / T 01021-1992)" and evaluate by the percentage of bacteria reduction.

[0136] Water absorption test: Refer to "GB / T 22799-2019 Test method for water absorption of towel products-Absorption method" for testing, and calculate the fabric's absorption rate of a certain amount of water to measure the fabric's hydrophilic and water absorption properties.

[0137] Hair loss rate test: refer to "GB / T 22798-2019 Test method for hair loss rate of towel products-water washing weight loss method", weigh the mass of the towel before and after finishing, and calculate the percentage of mass loss of the towel, which is the hair loss rate of the towel.

[0138] Table 2 Fabric performance test results using the silicone softener of this application

[0139]

[0140]

[0141] Analyzing the test performance evaluation results of the organic silicone softener for towels in Table 2, after the towels are treated with the organic silicone softener for towels of the present application, the feel, softness and water absorption rate of the towels are improved, making the towels have a better touch, softer and better water absorption. In addition, after the towels are treated with the organic silicone softener for towels of the present application, the towels are endowed with certain antibacterial properties, and the towels have a good inhibition rate on Escherichia coli and Staphylococcus aureus, thereby improving the hygiene and cleanliness of the towels.

[0142] In the preparation process of the organosilicon softener for towels, the addition amount, number average molecular weight and hydrogen content of the synthetic raw materials are adjusted, which has a certain influence on the performance of the towels after treatment. In the towel application test performance evaluation results of Example 7, the towels after treatment have the best comprehensive performance, with a 5-level hand feeling evaluation and a water holding rate of 73.57%, an Escherichia coli inhibition rate of 86.76% and a Staphylococcus aureus inhibition rate of 89.31%.

[0143] By analyzing Example 7, Example 9 and Example 10, the reaction time of step S2 or step S3 was adjusted, but the performance of the towel was not significantly improved. That is, the reaction time of Example 7 has allowed the raw materials to fully react and synthesize, and extending the reaction time cannot improve the product performance.

[0144] The towel application test performance evaluation results of Example 7 and Comparative Example 1 were analyzed. In the preparation process of Comparative Example 1, polyetheramine ED400 replaced polyether-modified imidazole for the synthesis reaction, so that the structure of the silicone softener of Comparative Example 1 after the reaction did not include an imidazole structure, and the towel treated with the silicone softener of Comparative Example 1 could only improve the hand feel, softness and water holding rate, but did not have antibacterial properties. In the silicone softener material structure for towels of the present application, the aminoimidazole structure can destroy the protection of bacteria by inhibiting the formation of biofilm, giving the towel treated with it certain antibacterial properties.

[0145] The test results of the hair loss rate of the towels of Example 7 and Comparative Examples 2, 3 and 4 were analyzed. The hair loss rates of Comparative Examples 2-4 were significantly higher than that of Example 7. The towels of Comparative Examples 2-4 after finishing could only be judged as first-class products according to the hair loss rates, while Example 7 could be judged as a superior product. This indicates that the presence of carboxylate reduces the cationicity of the product, reduces the repulsive force between fibers, and can effectively reduce the hair loss rate of the towels.

[0146] The treatment effects of the two commercially available silicone oils on towels, although the feel and water holding rate are improved, the softness and antibacterial rate are not as good as the silicone softener prepared in this application.

[0147] In summary, the organosilicon softener for towels provided in the present application has good stability, and after treatment, the towels are endowed with good hand feel, softness, antibacterial effect and water absorption. In addition, the preparation method of the organosilicon softener for towels is simple, the reaction process is controllable, and it is suitable for industrial production, and has certain practical application significance.

[0148] The above describes the basic principles, main features and advantages of the present application. Those skilled in the art should understand that the present application is not limited by the above embodiments, and the above embodiments and the specification only describe the principles of the present application. The present application may have various changes and improvements without departing from the spirit and scope of the present application, and these changes and improvements fall within the scope of the present application for which protection is sought. The scope of protection claimed by the present application is defined by the attached claims and their equivalents.

Claims

1. A silicone softener material for towels, characterized in that: Its general structural formula is: Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

2. A method for preparing a silicone softener material for towels, characterized in that: The method comprises the following preparation steps: S1: 2-aminoimidazole and polyethylene glycol diglycidyl ether are reacted in an organic solvent to prepare a polyether-modified imidazole; S2: preparing polyether modified silicone oil by catalytic reaction of side hydrogen-containing silicone oil and allyl polyoxyethylene glycidyl ether; S3: the polyether-modified imidazole, the polyether-modified silicone oil and the disodium glutamate aqueous solution are reacted to obtain the organic silicone softener material for towels after removing impurities; The general structural formula of the polyether-modified imidazole is: Where n is an integer, and 1≤n≤6; The general structural formula of the polyether modified silicone oil is: Wherein a, c, d, e, m are integers, and 0≤a≤263, 0≤c≤263, 1≤d≤5, 4≤e≤10, 9≤m≤20; The general structural formula of the organosilicon softener material for towels is: Where M is (CH2CH2O), R is a, c, d, e, f, g, m, n are integers; and 0≤a≤263, 0≤c≤263, 1≤d≤5, 9≤m≤20, 2≤f≤5, 2≤g≤5, 1≤n≤6.

3. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The number average molecular weight of the polyethylene glycol diglycidyl ether is 200-400.

4. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The number average molecular weight of the side hydrogen-containing silicone oil is 20000-30000, and the hydrogen content of the side hydrogen-containing silicone oil is 0.027%-0.05%.

5. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The number average molecular weight of the allyl polyoxyethylene ether glycidyl ether is 500-1000.

6. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The mass fraction of disodium glutamate in the disodium glutamate aqueous solution is 30% to 60%.

7. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The S1 step is specifically as follows, by mass: 166 parts of the 2-aminoimidazole and 366-566 parts of the organic solvent are added to a reaction device, stirred and heated, and after the 2-aminoimidazole is completely dissolved, 200-400 parts of the polyethylene glycol diglycidyl ether are slowly added to the reaction device, and the polyether-modified imidazole is obtained after keeping the temperature for 4-6 hours.

8. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The S2 step is specifically as follows, calculated by mass: 2000-3000 parts of the side hydrogenated silicone oil and 200-1000 parts of the allyl polyoxyethylene ether glycidyl ether are reacted in a reaction device, and then 940-1715 parts of an organic solvent and 2-3 parts of a catalyst are added to the reaction device, and the temperature is increased and kept to react for 6-8 hours to obtain the polyether-modified silicone oil.

9. The method for preparing the organosilicon softener material for towels according to claim 2, characterized in that: The S3 step is specifically as follows, calculated by mass: 3140 to 5715 parts of the polyether-modified silicone oil, 146 to 566 parts of the polyether-modified imidazole and 76 to 191 parts of the disodium glutamate aqueous solution are added to the reaction device, and then 1256 to 2285 parts of the organic solvent are added, the temperature is increased and kept for a period of time, and finally the impurities in the product are removed.

10. A silicone softener for towels, characterized in that: The invention is prepared from the following raw materials in parts by weight: 200 to 300 parts of deionized water, 2 to 4 parts of glacial acetic acid, 15 to 30 parts of emulsifier, and 80 to 120 parts of the organic silicone softener material for towels as claimed in claim 1, or the organic silicone softener material for towels prepared by the preparation method as claimed in claims 2 to 9.

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