Preparation method for air-permeable and antibacterial silicone rubber material and application thereof in home textiles
12466954 ยท 2025-11-11
Assignee
Inventors
Cpc classification
B29K2075/00
PERFORMING OPERATIONS; TRANSPORTING
Y02A50/30
GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
C08L83/08
CHEMISTRY; METALLURGY
B29C43/003
PERFORMING OPERATIONS; TRANSPORTING
C08L83/10
CHEMISTRY; METALLURGY
B29K2995/0077
PERFORMING OPERATIONS; TRANSPORTING
B29K2105/0005
PERFORMING OPERATIONS; TRANSPORTING
A01N55/00
HUMAN NECESSITIES
B29K2083/00
PERFORMING OPERATIONS; TRANSPORTING
C08L83/08
CHEMISTRY; METALLURGY
International classification
C08L83/10
CHEMISTRY; METALLURGY
A01N55/00
HUMAN NECESSITIES
Abstract
The present disclosure relates to the technical field of silicone rubbers, and discloses a preparation method for an air-permeable and antibacterial silicone rubber material and an application thereof in home textiles. Activated silicone rubber and double quaternary ammonium salt-type benzoic acid are subjected to an esterification reaction under the catalysis of p-toluenesulfonic acid to obtain double quaternary ammonium salt-grafted silicone rubber. The double quaternary ammonium salt-grafted silicone rubber is blended with silicone rubber and then applied to home textiles, wherein the quaternary ammonium salt component can destroy cellular enzymes in bacteria and has an antibacterial effect, and the silicon-oxygen-silicon in the silicone rubber not only has excellent air permeability, but also has excellent mechanical properties. Finally, the home textile material with excellent antibacterial properties, air permeability and mechanical properties is obtained.
Claims
1. A preparation method for an air-permeable and antibacterial silicone rubber material, wherein the silicone rubber material consists of the following components in parts by weight: 50-70 parts by weight of a double quaternary ammonium salt-grafted silicone rubber, 30-50 parts by weight of a polyurethane elastomer, 1-2 parts by weight of a compatibilizer, and 0.5-1 parts by weight of a vulcanizing agent; and wherein the air-permeable and antibacterial silicone rubber material is prepared by the following steps: (1) placing an activated silicone rubber, a double quaternary ammonium salt-type benzoic acid and a p-toluenesulfonic acid catalyst in a first reaction kettle filled with a toluene solvent, reacting the activated silicone rubber with the double quaternary ammonium salt-type benzoic acid at 70-90 C. for 5-10 h to obtain a first reaction product, washing the first reaction product with deionized water, and drying the first reaction product to obtain the double quaternary ammonium salt-grafted silicone rubber; and (2) at 180-200 C., placing the double quaternary ammonium salt-grafted silicone rubber, the polyurethane elastomer, the compatibilizer and the vulcanizing agent in a torque rheometer with a rotating speed of 50-80 r/min to form a mixture, blending the mixture for 10-20 min, cooling the blended mixture to room temperature, and performing vulcanization and compression molding on the cooled mixture in a flat vulcanizing machine with a pressure of 10-12 MPa to obtain the air-permeable and antibacterial silicone rubber material.
2. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 1, wherein a ratio of the activated silicone rubber in parts by weight to the double quaternary ammonium salt-type benzoic acid in parts by weight to the p-toluenesulfonic acid catalyst in parts by weight in the step (2) is 100:400-500:10-30.
3. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 1, wherein the vulcanization in the step (2) is performed as follows: a primary vulcanization is performed at 170-190 C. for 5-15 min, and a secondary vulcanization is performed in an oven at 200-220 C. for 4-8 h.
4. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 1, wherein a preparation method for the double quaternary ammonium salt-type benzoic acid in the step (1) is as follows: (3) stirring and dissolving 3,5-dichlorobenzaldehyde in a second reaction kettle filled with an acetone solvent, adding and uniformly stirring a solution of 4-vinylphenol in acetone into the second reaction kettle at 50-60 C., refluxing to form a second reaction product of the 3,5-dichlorobenzaldehyde with the 4-vinylphenol for 15-25 h, filtrating the second reaction product in vacuum, washing the second reaction product with deionized water and acetone in sequence, and drying the second reaction product to obtain a distyryl benzaldehyde intermediate; (4) placing and stirring for dissolving the distyryl benzaldehyde intermediate into a third reaction kettle filled with an acetic acid solvent, adding a potassium bromide oxidant into the third reaction kettle at 80-100 C. and stirring for 1-3 h to form a third reaction product of the distyryl benzaldehyde intermediate with the potassium bromide oxidant, cooling the third reaction product to room temperature, filtrating the third reaction product in vacuum, washing the third reaction product with deionized water, recrystallizing the third reaction product with ethanol, and drying the third reaction product to obtain a distyryl benzoic acid intermediate; (5) dissolving the distyryl benzoic acid intermediate in a fourth reaction kettle filled with a dichloromethane solvent, adding m-chloroperoxybenzoic acid into the fourth reaction kettle at 0-5 C. and stirring and mixing in the fourth reaction kettle for 2-5 h, heating to room temperature and reacting the distyryl benzoic acid with the m-chloroperoxybenzoic acid for 15-30 h to form a fourth reaction product, washing the fourth reaction product with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and drying the fourth reaction product to obtain a diphenyl epoxy benzoic acid intermediate; and (6) dissolving the diphenyl epoxy benzoic acid intermediate in a fifth reaction kettle filled with an absolute ethanol solvent, adding N,N-dimethylethylamine into the fifth reaction kettle and stirring for reaction of the diphenyl epoxy benzoic acid intermediate with the N,N-dimethylethylamine for 20-40 h to form a fifth reaction product, distilling the fifth reaction product under a reduced pressure, washing the fifth reaction product with acetone, and drying the fifth reaction product to obtain the double quaternary ammonium salt-type benzoic acid.
5. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 4, wherein a molar ratio of the 3,5-dichlorobenzaldehyde to the 4-vinylphenol in the step (3) is 1:2-2.5.
6. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 4, wherein a molar ratio of the distyryl benzaldehyde intermediate to the potassium bromide oxidant in the step (4) is 1:0.3-0.5.
7. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 4, wherein a molar ratio of the distyryl benzoic acid intermediate to the m-chloroperoxybenzoic acid in the step (5) is 1:2-4.
8. The preparation method for an air-permeable and antibacterial silicone rubber material according to claim 4, wherein a molar ratio of the diphenyl epoxy benzoic acid intermediate to the N,N-dimethylethylamine in the step (6) is 1:2-2.5.
9. A method of applying the air-permeable and antibacterial silicone rubber material prepared by the preparation method according to claim 1 in home textiles comprising placing the prepared air-permeable and antibacterial silicone rubber material in a cover body of a home textile material to obtain a home textile material containing a silicone rubber core.
Description
BRIEF DESCRIPTION OF DRAWINGS
(1) FIGURE shows a preparation route of double quaternary ammonium salt-type benzoic acid.
DETAILED DESCRIPTION OF EMBODIMENTS
(2) To make the objectives, embodiments and advantages of the present application clearer, the following clearly and completely describes exemplary embodiments of the present application with reference to the accompanying drawings in the exemplary embodiments of the present application. It is clear that the described exemplary embodiments are merely some rather than all of embodiments of the present application.
(3) It should be noted that the brief descriptions of the terms in the present application are only for the convenience of understanding the embodiments described below, and are not intended to limit the embodiments of the present application. These terms should be understood according to ordinary and common meaning unless otherwise specified.
(4) The preparation method for the activated silicone rubber comprises: cutting up silicone rubber, placing in absolute alcohol for cleaning, after drying, placing the silicone rubber in a methanol solution of potassium hydroxide with a mass fraction of 1%, stirring and soaking at 50 C. for 40-80 min, and washing with methanol to obtain the activated silicone rubber.
(5) The compatilizer is KH550, and the vulcanizing agent is a bis-2,5 vulcanizing agent.
(6) The silicone rubber material of the present disclosure is prepared by the following preparation steps of examples and comparative examples.
Example 1
(7) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving. An acetone solution containing 0.4 mol of 4-vinylphenol was added into the reaction kettle at 55 C., stirred uniformly, refluxed for reaction for 25 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(8) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving. 0.015 mol of potassium bromide oxidant was added into the reaction kettle at 90 C., stirred for reaction for 3 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyrylbenzoic acid intermediate.
(9) S3: 0.06 mol of the distyrylbenzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent. 0.2 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 5 C., stirred and mixed for 3 h, heated to the room temperature, reacted for 20 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(10) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.2 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(11) S5: 100 parts by weight of the activated silicone rubber, 400 parts by weight of the double quaternary ammonium salt-type benzoic acid and 20 parts by weight of p-toluenesulfonic acid catalyst were placed in a reaction kettle filled with a toluene solvent, reacted at 80 C. for 8 h, washed with deionized water after the reaction was completed, and dried to obtain double quaternary ammonium salt-grafted silicone rubber.
(12) S6: at 200 C., 30 parts by weight of the double quaternary ammonium salt-grafted silicone rubber, 70 parts by weight of the polyurethane elastomer, 2 parts by weight of the compatilizer and 0.5 parts by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 60 r/min, blended for 15 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 12 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 180 C. for 10 min, and a secondary vulcanization was performed in an oven at 220 C. for 6 h, and finally the air-permeable and antibacterial silicone rubber material was obtained.
Example 2
(13) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving, an acetone solution containing 0.5 mol of 4-vinylphenol was added into the reaction kettle at 50 C., stirred uniformly, refluxed for reaction for 20 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(14) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving, 0.015 mol of potassium bromide oxidant was added into the reaction kettle at 90 C., stirred for reaction for 3 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyryl benzoic acid intermediate.
(15) S3: 0.06 mol of the distyryl benzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent, 0.15 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 0 C., stirred and mixed for 4 h, heated to the room temperature, reacted for 20 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(16) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.2 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(17) S5: 100 parts by weight of the activated silicone rubber, 450 parts by weight of the double quaternary ammonium salt-type benzoic acid and 25 parts by weight of p-toluenesulfonic acid catalyst were placed in a reaction kettle filled with a toluene solvent, reacted at 80 C. for 6 h, washed with deionized water after the reaction was completed, and dried to obtain double quaternary ammonium salt-grafted silicone rubber.
(18) S6: at 190 C., 35 parts by weight of the double quaternary ammonium salt-grafted silicone rubber, 65 parts by weight of the polyurethane elastomer, 2 parts by weight of the compatilizer and 0.5 parts by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 70 r/min, blended for 10 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 11 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 180 C. for 10 min, and a secondary vulcanization was performed in an oven at 210 C. for 6 h, and finally the air-permeable and antibacterial silicone rubber material was obtained.
Example 3
(19) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving, an acetone solution containing 0.45 mol of 4-vinylphenol was added into the reaction kettle at 55 C., stirred uniformly, refluxed for reaction for 20 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(20) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving, 0.025 mol of potassium bromide oxidant was added into the reaction kettle at 80 C., stirred for reaction for 2 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyryl benzoic acid intermediate.
(21) S3: 0.06 mol of the distyryl benzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent, 0.24 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 3 C., stirred and mixed for 2 h, heated to the room temperature, reacted for 20 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(22) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.2 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(23) S5: 100 parts by weight of the activated silicone rubber, 480 parts by weight of the double quaternary ammonium salt-type benzoic acid and 20 parts by weight of p-toluenesulfonic acid catalyst were placed in a reaction kettle filled with a toluene solvent, reacted at 80 C. for 8 h, washed with deionized water after the reaction was completed, and dried to obtain double quaternary ammonium salt-grafted silicone rubber.
(24) S6: at 190 C., 40 parts by weight of the double quaternary ammonium salt-grafted silicone rubber, 60 parts by weight of the polyurethane elastomer, 2 parts by weight of the compatilizer and 0.5 parts by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 70 r/min, blended for 10 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 12 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 180 C. for 15 min, and a secondary vulcanization was performed in an oven at 200 C. for 6 h, and finally the air-permeable and antibacterial silicone rubber material was obtained.
Example 4
(25) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving, an acetone solution containing 0.5 mol of 4-vinylphenol was added into the reaction kettle at 60 C., stirred uniformly, refluxed for reaction for 15 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(26) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving, 0.015 mol of potassium bromide oxidant was added into the reaction kettle at 90 C., stirred for reaction for 3 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyryl benzoic acid intermediate.
(27) S3: 0.06 mol of the distyryl benzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent, 0.2 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 0 C., stirred and mixed for 5 h, heated to the room temperature, reacted for 15 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(28) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.2 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(29) S5: 100 parts by weight of the activated silicone rubber, 500 parts by weight of the double quaternary ammonium salt-type benzoic acid and 10 parts by weight of p-toluenesulfonic acid catalyst were placed in a reaction kettle filled with a toluene solvent, reacted at 80 C. for 8 h, washed with deionized water after the reaction was completed, and dried to obtain double quaternary ammonium salt-grafted silicone rubber.
(30) S6: at 190 C., 45 parts by weight of the double quaternary ammonium salt-grafted silicone rubber, 55 parts by weight of the polyurethane elastomer, 1 part by weight of the compatilizer and 1 part by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 80 r/min, blended for 15 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 12 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 170 C. for 10 min, and a secondary vulcanization was performed in an oven at 210 C. for 7 h, and finally the air-permeable and antibacterial silicone rubber material was obtained.
Example 5
(31) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving, an acetone solution containing 0.45 mol of 4-vinylphenol was added into the reaction kettle at 55 C., stirred uniformly, refluxed for reaction for 15 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(32) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving, 0.015 mol of potassium bromide oxidant was added into the reaction kettle at 100 C., stirred for reaction for 3 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyryl benzoic acid intermediate.
(33) S3: 0.06 mol of the distyryl benzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent, 0.24 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 0 C., stirred and mixed for 4 h, heated to the room temperature, reacted for 20 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(34) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.16 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(35) S5: 100 parts by weight of the activated silicone rubber, 500 parts by weight of the double quaternary ammonium salt-type benzoic acid and 30 parts by weight of p-toluenesulfonic acid catalyst were placed in a reaction kettle filled with a toluene solvent, reacted at 80 C. for 8 h, washed with deionized water after the reaction was completed, and dried to obtain double quaternary ammonium salt-grafted silicone rubber.
(36) S6: at 190 C., 50 parts by weight of the double quaternary ammonium salt-grafted silicone rubber, 50 parts by weight of the polyurethane elastomer, 1 part by weight of the compatilizer and 1 part by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 80 r/min, blended for 15 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 11 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 190 C. for 5 min, and a secondary vulcanization was performed in an oven at 210 C. for 5 h, and finally the air-permeable and antibacterial silicone rubber material was obtained.
Comparative Example 1
(37) S1: at 200 C., 30 parts by weight of the activated silicone rubber, 70 parts by weight of the polyurethane elastomer, 2 parts by weight of the compatilizer and 0.5 parts by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 60 r/min, blended for 15 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 12 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 180 C. for 10 min, and a secondary vulcanization was performed in an oven at 220 C. for 6 h, and finally the silicone rubber material was obtained.
Comparative Example 2
(38) S1: 0.2 mol of 3,5-dichlorobenzaldehyde was dissolved in a reaction kettle filled with an acetone solvent, stirred for dissolving, an acetone solution containing 0.4 mol of 4-vinylphenol was added into the reaction kettle at 55 C., stirred uniformly, refluxed for reaction for 25 h, after the reaction was completed, filtrated in vacuum, washed with deionized water and acetone in sequence, and dried to obtain a distyryl benzaldehyde intermediate.
(39) S2: 0.03 mol of the distyryl benzaldehyde intermediate was placed into a reaction kettle filled with an acetic acid solvent, stirred for dissolving, 0.015 mol of potassium bromide oxidant was added into the reaction kettle at 90 C., stirred for reaction for 3 h, cooled to the room temperature after the reaction was completed, filtrated in vacuum, washed with deionized water, recrystallized with ethanol, and dried to obtain a distyryl benzoic acid intermediate.
(40) S3: 0.06 mol of the distyryl benzoic acid intermediate was dissolved in a reaction kettle filled with a dichloromethane solvent, 0.2 mol of m-chloroperoxybenzoic acid was added into the reaction kettle at 5 C., stirred and mixed for 3 h, heated to the room temperature, reacted for 20 h, after the reaction was completed, washed with a saturated sodium bicarbonate solution and a saturated saline solution in sequence, and dried to obtain a diphenyl epoxy benzoic acid intermediate.
(41) S4: 0.08 mol of the diphenyl epoxy benzoic acid intermediate was dissolved in a reaction kettle filled with an absolute ethanol solvent, 0.2 mol of N,N-dimethylethylamine was added into the reaction kettle, stirred for reaction for 30 h, distilled under a reduced pressure, washed with acetone, and dried to obtain the double quaternary ammonium salt-type benzoic acid.
(42) S5: at 200 C., 30 parts by weight of the double quaternary ammonium salt-type benzoic acid, 70 parts by weight of the polyurethane elastomer, 2 parts by weight of the compatilizer and 0.5 parts by weight of the vulcanizing agent were placed in a torque rheometer with a rotating speed of 60 r/min, blended for 15 min, cooled to the room temperature after the blending was completed, and compression molding was performed in a flat vulcanizing machine with a pressure of 12 MPa, wherein the vulcanization was as follows: a primary vulcanization was performed at 180 C. for 10 min, and a secondary vulcanization was performed in an oven at 220 C. for 6 h, and finally the silicone rubber material was obtained.
(43) The silicone rubber materials obtained from Examples and Comparative Examples were subjected to the following tests.
(44) Antibacterial performance test: the dried and sterilized silicone rubber material was placed into a phosphoric acid buffer solution, the phosphoric acid buffer solution without the silicone rubber material was taken as a blank control sample, inoculated with Escherichia coli, shaked and contacted for 12 h. 1 mL of the shaked bacterial liquid was added into a culture dish, cultured for 36 h at 37 C., the number of bacteria was determined, and the bacteriostatic rate was calculated, wherein Y=(AB)/A100%.
(45) The test results are shown in the table below:
(46) TABLE-US-00001 A (CFU/mL) B (CFU/mL) Y (%) Example 1 3.85 10.sup.7 3.71 10.sup.7 96.4 Example 2 3.85 10.sup.7 3.78 10.sup.7 98.2 Example 3 3.85 10.sup.7 3.81 10.sup.7 90.0 Example 4 3.85 10.sup.7 3.82 10.sup.7 99.2 Example 5 3.85 10.sup.7 3.84 10.sup.7 99.7 Comparative 3.85 10.sup.7 0.96 10.sup.7 24.9 Example 1 Comparative 3.85 10.sup.7 3.72 10.sup.7 96.6 Example 2 A is the number of viable bacteria (CFU/mL) after the blank sample comes into contact with bacteria. B is the number of viable bacteria (CFU/mL) after the sample comes into contact with bacteria. Y is the bacteriostatic rate.
(47) The antibacterial effects of Examples 1-5 and Comparative Example 2 are better, and the antibacterial effect of Comparative Example 1 is poor. This is because the double quaternary ammonium salt component is contained in Examples 1-5 and Comparative Example 2, and the quaternary ammonium salt has a broad-spectrum sterilization effect and can enter bacterial cells to passivate the cells, so that bacteriostasis and sterilization are achieved. In Comparative Example 1, no quaternary ammonium salt was added, and thus the antibacterial effect was the worst.
(48) The tensile strength of the silicone rubber material was tested using a universal tester. The stretching rate was 500 mm/min.
(49) The Shore A hardness of silicone rubber material was tested using a Shore A hardness tester.
(50) The test results are shown in the table below:
(51) TABLE-US-00002 Elongation at break Tensile strength/MPa (%) Hardness Example 1 3.54 206 60 Example 2 3.90 258 65 Example 3 4.36 314 72 Example 4 4.81 264 68 Example 5 4.46 213 63 Comparative 3.56 211 59 Example 1 Comparative 2.67 183 46 Example 2
(52) The mechanical properties of Examples 1-5 and Comparative Example 1 are better than those of Comparative Example 2. This is because the activated silicone rubber with larger silicon-oxygen bond energy is added in Examples 1-5 and Comparative Example 1, and because the silicon-oxygen-silicon chains are flexible and are cross-linked and wound with each other to form a huge network structure, the energy suffered by the silicone rubber material can be transferred when the silicone rubber material is impacted, so that the mechanical properties of the silicone rubber material are improved. The prepared double quaternary ammonium salt-type benzoic acid that is added in Comparative Example 2 is a small molecular structure, and the accumulated and superposed benzene ring structures and hydrogen bonds of this small molecular structure can also transfer the impact energy suffered by the silicone rubber material; however, the above is inferior to the mechanical properties brought by the silicone rubber, so the mechanical properties of Comparative Example 2 are poor.
(53) The air permeability of the silicone rubber material was tested using an oxygen transmission rate tester.
(54) TABLE-US-00003 Oxygen transmission rate/cm.sup.3 (m.sup.2 .Math. d .Math. Pa).sup.1 Example 1 369.237 Example 2 308.116 Example 3 223.889 Example 4 158.434 Example 5 178.691 Comparative Example 1 396.145 Comparative Example 2 462.336
(55) The oxygen transmission rate of Examples 1-5 and Comparative Example 1 is lower than that of Comparative Example 2, and thus the air permeability of Examples 1-5 and Comparative Example 1 is better than that of Comparative Example 2. This is because the silicone rubber having a silicon-oxygen-silicon chain is added to Examples 1-5 and Comparative Example 1, and the silicon-oxygen-silicon chain is a flexible chain that is easy to rotate and has a low cohesive energy density, and the amorphous aggregate state has a large free volume. Therefore, Examples 1-5 and Comparative Example 1 have a large air permeability, and while Comparative Example 2 has no silicone rubber added thereto and thus has a poor air permeability.
(56) In conclusion, the air-permeable and antibacterial silicone rubber material prepared in the solutions of the present disclosure has both better antibacterial performance and a better air permeability.
(57) The above embodiments are provided only for illustrating the present disclosure and not for limiting the present disclosure. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, therefore all equivalent technical solutions should also fall into the scope of the present disclosure, and should be defined by the claims.