Slow-resilience silica gel pillow and preparation method thereof

Abstract

The invention relates to the technical field of household articles, in particular to a slow-rebound silica gel pillow and a preparation method thereof, which are used for solving the problems that the existing slow-rebound pillow is easy to generate peculiar smell, the hardness is difficult to adjust, and the existing slow-rebound pillow is easy to deform, easy to breed bacteria and difficult to clean and maintain in long-term use. The pillow adopts silica gel as a slow-rebound material, does not generate peculiar smell, has good pressure dispersing capacity, effectively relieves neck pressure, promotes blood circulation during sleeping, improves sleeping quality, ensures durability and stability of the pillow inner, is not prone to deformation and aging, and is long in service life. After the modified organic silicon is added, the softness, resilience and comfort of the pillow can be further improved, meanwhile, the antibacterial and bacteriostatic performance of the pillow is remarkably improved, the growth of bacteria and mites is effectively inhibited, the health of a user is protected, the pillow case is detachable, the pillow inner can be cleaned and easily dried, and the pillow is kept clean and tidy.

Description

Technical Field

[0001] The invention relates to the technical field of household products, and in particular to a slow-rebound silica gel pillow and a preparation method thereof. Background Art

[0002] As people's living standards improve, their requirements for sleep quality are getting higher and higher. Pillows are important items during sleep, and their performance directly affects people's sleep comfort. Traditional pillow materials such as cotton and down have certain limitations in terms of support, breathability and resilience. Slow-rebound materials have gradually attracted attention because of their ability to produce corresponding deformations according to human body pressure and slowly return to their original state after the pressure disappears. However, most of the materials of existing slow-rebound pillows are polyurethane foam materials, which have environmental problems, are prone to odor, and are difficult to adjust in hardness. In addition, they are easy to deform, easy to breed bacteria, and difficult to clean and maintain during long-term use.

[0003] In view of this, it is of great significance to study and develop a slow-rebound silica gel pillow and a preparation method thereof. In view of the above technical defects, a solution is now proposed. Summary of the invention

[0004] In order to overcome the above-mentioned technical problems, the purpose of the present invention is to provide a slow-rebound silicone pillow and a preparation method thereof, which solves the problems that the existing slow-rebound pillows are prone to produce odor, are difficult to adjust the hardness, are easy to deform, easy to breed bacteria, and are difficult to clean and maintain during long-term use.

[0005] The purpose of the present invention can be achieved by the following technical solutions:

[0006] A slow-rebound silicone pillow comprising a cotton pillowcase and a silicone pillow core

[0007] Wherein, the silica gel pillow core comprises the following components in parts by weight:

[0008] 60-70 parts of silica gel, 11-35 parts of modified organic silicon, 7-11 parts of nano silicon dioxide, 5-9 parts of nano titanium dioxide, 0.2-0.3 parts of sodium bicarbonate, 0.1-0.2 parts of sodium dodecyl sulfate, 1-3 parts of sodium carboxymethyl cellulose, 0.3-0.5 parts of dibenzothiazole disulfide and 40-60 parts of acetic acid solution.

[0009] As a further solution of the present invention: the modified silicone is prepared by the following steps:

[0010] Step s1: sodium hydroxide, deionized water and anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for reaction for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400 r / min, then diethylamine is added and the temperature is raised to 45-50°C and the stirring reaction is continued for 20-30 minutes, then 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 1-2 drops / s, and after the dropwise addition is completed, the temperature is raised to 60-65°C and the stirring reaction is continued for 8-10 hours, and after the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate 2-3 times, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate;

[0011] Step s2: 1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a reflux condenser, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 30-40 min, and then the temperature is raised to 120-130° C. and the stirring reaction is continued for 5-6 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0012] Step s3: Add the olefinic intermediate, the terminal hydrogen intermediate, chloroplatinic acid and anhydrous acetone into a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, introduce nitrogen protection, stir the reaction at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 min, then heat the temperature to 40-50° C. and continue stirring the reaction for 2-3 h. After the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent to obtain a terminal tertiary amine intermediate;

[0013] Step s4: Add the terminal tertiary amine intermediate, monobromododecane, anhydrous potassium carbonate and anhydrous acetone into a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir the reaction at a temperature of 25-30°C and a stirring rate of 300-400r / min for 30-40min, then raise the temperature to 85-90°C and continue stirring the reaction for 15-20h. After the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent, then wash with petroleum ether and distilled water for 3-5 times in turn, then place it in a vacuum drying oven, and dry it at a temperature of 50-55°C for 3-5h to obtain modified silicone.

[0014] As a further scheme of the present invention: the usage ratio of the sodium hydroxide, deionized water, anhydrous ether, diethylamine and 3-bromo-1-propylene in step s1 is 2-5 g: 20-25 mL: 40-45 mL: 22-25 mmol: 10 mmol.

[0015] As a further solution of the present invention: the usage ratio of the 1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane and toluene in step s2 is 10-20 mmol:50 mmol:60-70 mL.

[0016] As a further solution of the present invention: the usage ratio of the alkenyl intermediate, the terminal hydrogen intermediate, chloroplatinic acid and anhydrous acetone in step s3 is 1.5-5.5 g: 10 g: 0.01-0.03 g: 60-70 mL.

[0017] As a further solution of the present invention: the usage ratio of the terminal tertiary amine intermediate, monobromododecane, anhydrous potassium carbonate and anhydrous acetone in step s4 is 10g:1.3-3.9g:4-6g:70-80mL.

[0018] As a further solution of the present invention: a method for preparing a slow-rebound silica gel pillow comprises the following steps:

[0019] Step 1: Weigh 60-70 parts of silica gel, 11-35 parts of modified silicone, 7-11 parts of nano silicon dioxide, 5-9 parts of nano titanium dioxide, 0.2-0.3 parts of sodium bicarbonate, 0.1-0.2 parts of sodium dodecyl sulfate, 1-3 parts of sodium carboxymethyl cellulose, 0.3-0.5 parts of dibenzothiazole disulfide and 40-60 parts of acetic acid solution according to weight parts, and set aside;

[0020] Step 2: Add silica gel, modified silicone, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stir evenly, then add into an open mill, mix at a mixing temperature of 90-120° C. for 15-20 minutes to obtain a film;

[0021] Step 3: Crush the film and place it in an oven, vulcanize it at a temperature of 150-160°C for 10-15 minutes, then melt it through an extruder into a pillow mold, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0022] As a further solution of the present invention: the mass fraction of the acetic acid solution is 2-3%.

[0023] Beneficial effects of the present invention:

[0024] The invention discloses a slow-rebound silicone pillow and a preparation method thereof. The method comprises the following steps: uniformly stirring silicone, modified organic silicon, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution, and then kneading to obtain a film. The film is then crushed and vulcanized, and then extruded into a pillow mold for curing to obtain a silicone pillow core. The silicone pillow core is then loaded into a cotton pillowcase to obtain a slow-rebound silicone pillow. The pillow adopts silicone as a slow-rebound material. Silica gel is a new type of environmentally friendly material, and its flexibility, acid and alkali resistance and high temperature resistance are better than those of polyurethane. Urethane, and does not produce odor, and has good pressure dispersion ability. It can adaptively adjust according to the shape and pressure distribution of the human head and neck, provide uniform support, effectively relieve neck pressure, promote blood circulation during sleep, improve sleep quality, and ensure the durability and stability of the pillow core. It is not easy to deform or age, and has a long service life. Adding modified silicone to it can further improve its softness, resilience and comfort, and significantly improve its antibacterial and antibacterial properties, effectively inhibit the growth of bacteria and mites, and protect the health of users. The pillowcase is detachable and the pillow core is washable and easy to dry to keep the pillow clean.

[0025] In the process of preparing the slow-rebound silicone pillow, a modified organic silicon is first prepared. First, diethylamine and 3-bromo-1-propylene are reacted, and the secondary amine group on the diethylamine reacts with the bromine on the 3-bromo-1-propylene to obtain an alkenyl intermediate containing a tertiary amine group and an alkenyl group. Then, 1,1,3,3-tetramethyldisiloxane and octamethylcyclotetrasiloxane are polymerized to form an organic silicon containing a hydrogen atom at the end to obtain a terminal hydrogen intermediate. Then, the alkenyl intermediate and the terminal hydrogen intermediate react, and the alkenyl on the alkenyl intermediate reacts with the Si-H bond on the terminal hydrogen intermediate to obtain a terminal tertiary amine intermediate. Finally, the terminal The tertiary amine intermediate and monobromododecane react, and the tertiary amine group on the terminal tertiary amine intermediate reacts with the bromine atom on the monobromododecane to form a quaternary ammonium group, thereby obtaining a modified silicone. The silicone material has excellent softness and low surface energy. Adding it to the pillow core can further improve the comfort of the pillow core and give the pillow core good self-cleaning performance, which is easy to clean. At the same time, the modified silicone also contains a large number of quaternary ammonium groups. The quaternary ammonium groups are positively charged and can be adsorbed onto the negatively charged bacterial cell membrane, thereby destroying the bacterial cell membrane and inactivating the bacteria, giving it excellent antibacterial and antibacterial properties, thereby preventing bacteria from growing and affecting human health. DETAILED DESCRIPTION

[0026] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Embodiment 1:

[0028] This embodiment is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0029] Step S1: 2 g of sodium hydroxide, 20 mL of deionized water and 40 mL of anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for 20 min at a temperature of 25 ° C and a stirring rate of 300 r / min, then 22 mmol of diethylamine is added and the temperature is raised to 45 ° C and the stirring reaction is continued for 20 min, then 10 mmol of 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 1 drop / s. After the dropwise addition is completed, the temperature is raised to 60 ° C and the stirring reaction is continued for 8 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate twice, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate;

[0030] Step S2: 10 mmol 1,1,3,3-tetramethyldisiloxane, 50 mmol octamethylcyclotetrasiloxane, 60 mL and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen is introduced for protection. The reaction is stirred at a temperature of 25° C. and a stirring rate of 300 r / min for 30 min, and then the temperature is raised to 120° C. and the stirring reaction is continued for 5 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0031] Step S3: 1.5 g of the olefin intermediate, 10 g of the terminal hydrogen intermediate, 0.01 g of chloroplatinic acid and 60 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at 25° C. and a stirring rate of 300 r / min for 20 min, and then the mixture was heated to 40° C. and the stirring reaction was continued for 2 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain a terminal tertiary amine intermediate;

[0032] Step S4: 10 g of the terminal tertiary amine intermediate, 1.3 g of monobromododecane, 4 g of anhydrous potassium carbonate and 70 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 25° C. and a stirring rate of 300 r / min for 30 min, and then the mixture was heated to 85° C. and the stirring reaction was continued for 15 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The mixture was then washed with petroleum ether and distilled water for 3 times in sequence, and then placed in a vacuum drying oven and dried at 50° C. for 3 h to obtain modified silicone;

[0033] Step S5: weigh 60 parts of silica gel, 11 parts of modified organosilicon, 7 parts of nano silicon dioxide, 5 parts of nano titanium dioxide, 0.2 parts of sodium bicarbonate, 0.1 parts of sodium dodecyl sulfate, 1 part of sodium carboxymethyl cellulose, 0.3 parts of dibenzothiazole disulfide and 40 parts of acetic acid solution with a mass fraction of 2% according to weight, and set aside;

[0034] Step S6: adding silica gel, modified organic silicon, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 90° C. for 15 minutes to obtain a film;

[0035] Step S7: Crush the film and place it in an oven, vulcanize it at 150°C for 10 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0036] Embodiment 2:

[0037] This embodiment is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0038] Step S1: 3.5 g of sodium hydroxide, 22 mL of deionized water and 42 mL of anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for reaction for 25 min at a temperature of 28 ° C and a stirring rate of 350 r / min, then 24 mmol of diethylamine is added and the temperature is raised to 48 ° C and the stirring reaction is continued for 25 min, then 10 mmol of 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 1 drop / s. After the dropwise addition is completed, the temperature is raised to 62 ° C and the stirring reaction is continued for 9 h. After the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate twice, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate;

[0039] Step S2: 15 mmol 1,1,3,3-tetramethyldisiloxane, 50 mmol octamethylcyclotetrasiloxane, 65 mL and toluene were added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen was introduced for protection. The reaction was stirred at a temperature of 28° C. and a stirring rate of 350 r / min for 35 minutes, and then the temperature was raised to 125° C. and the stirring reaction was continued for 5.5 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0040] Step S3: 3.5 g of the olefin intermediate, 10 g of the terminal hydrogen intermediate, 0.02 g of chloroplatinic acid and 65 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at 28° C. and a stirring rate of 350 r / min for 25 min, and then the mixture was heated to 45° C. and the stirring reaction was continued for 2.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain a terminal tertiary amine intermediate;

[0041] Step S4: 10 g of the terminal tertiary amine intermediate, 2.6 g of monobromododecane, 5 g of anhydrous potassium carbonate and 75 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 28° C. and a stirring rate of 350 r / min for 35 min, and then the mixture was heated to 88° C. and the stirring reaction was continued for 18 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The mixture was then washed with petroleum ether and distilled water for 4 times in sequence, and then placed in a vacuum drying oven and dried at 52° C. for 4 h to obtain modified silicone;

[0042] Step S5: weigh 65 parts of silica gel, 23 parts of modified organosilicon, 9 parts of nano silicon dioxide, 7 parts of nano titanium dioxide, 0.25 parts of sodium bicarbonate, 0.15 parts of sodium dodecyl sulfate, 2 parts of sodium carboxymethyl cellulose, 0.4 parts of dibenzothiazole disulfide and 50 parts of acetic acid solution with a mass fraction of 2.5% according to weight parts, and set aside;

[0043] Step S6: adding silica gel, modified organic silicon, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 105° C. for 18 minutes, to obtain a film;

[0044] Step S7: Crush the film and place it in an oven, vulcanize it at 155°C for 12 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0045] Embodiment 3:

[0046] This embodiment is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0047] Step S1: 5 g of sodium hydroxide, 25 mL of deionized water and 45 mL of anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, then 25 mmol of diethylamine is added and the temperature is raised to 50 ° C and the stirring reaction is continued for 30 min, then 10 mmol of 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 2 drops / s. After the dropwise addition is completed, the temperature is raised to 65 ° C and the stirring reaction is continued for 10 h. After the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate for 3 times, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate;

[0048] Step S2: 20 mmol 1,1,3,3-tetramethyldisiloxane, 50 mmol octamethylcyclotetrasiloxane, 70 mL and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen is introduced for protection. The reaction is stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 40 minutes, and then the temperature is raised to 130° C. and the stirring reaction is continued for 6 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0049] Step S3: 5.5 g of the olefin intermediate, 10 g of the terminal hydrogen intermediate, 0.03 g of chloroplatinic acid and 70 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at 30° C. and a stirring rate of 400 r / min for 30 min, and then the mixture was heated to 50° C. and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain a terminal tertiary amine intermediate;

[0050] Step S4: 10 g of the terminal tertiary amine intermediate, 3.9 g of monobromododecane, 6 g of anhydrous potassium carbonate and 80 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 30° C. and a stirring rate of 400 r / min for 40 min, and then the mixture was heated to 90° C. and stirred for 20 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The mixture was then washed with petroleum ether and distilled water for 5 times in sequence, and then placed in a vacuum drying oven and dried at 55° C. for 5 h to obtain modified silicone;

[0051] Step S5: weigh 70 parts of silica gel, 35 parts of modified organic silicon, 11 parts of nano silicon dioxide, 9 parts of nano titanium dioxide, 0.3 parts of sodium bicarbonate, 0.2 parts of sodium dodecyl sulfate, 3 parts of sodium carboxymethyl cellulose, 0.5 parts of dibenzothiazole disulfide and 60 parts of acetic acid solution with a mass fraction of 3% according to weight parts, and set aside;

[0052] Step S6: adding silica gel, modified organic silicon, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 120° C. for 20 minutes, to obtain a film;

[0053] Step S7: Crush the film and place it in an oven, vulcanize it at 160°C for 15 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0054] Comparative Example 1:

[0055] This comparative example is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0056] Step S1: weigh 70 parts of silica gel, 11 parts of nano silicon dioxide, 9 parts of nano titanium dioxide, 0.3 parts of sodium bicarbonate, 0.2 parts of sodium dodecyl sulfate, 3 parts of sodium carboxymethyl cellulose, 0.5 parts of dibenzothiazole disulfide and 60 parts of acetic acid solution with a mass fraction of 3% according to weight parts, and set aside;

[0057] Step S2: adding silica gel, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 120° C. for 20 minutes, to obtain a film;

[0058] Step S3: Crush the film and place it in an oven, vulcanize it at 160°C for 15 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0059] Comparative Example 2:

[0060] This comparative example is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0061] Step S1: 20 mmol 1,1,3,3-tetramethyldisiloxane, 50 mmol octamethylcyclotetrasiloxane, 70 mL and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen is introduced for protection. The reaction is stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 40 minutes, and then the temperature is raised to 130° C. and the stirring reaction is continued for 6 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0062] Step S2: 70 parts of silica gel, 35 parts of hydrogen-terminated intermediate, 11 parts of nano-silicon dioxide, 9 parts of nano-titanium dioxide, 0.3 parts of sodium bicarbonate, 0.2 parts of sodium dodecyl sulfate, 3 parts of sodium carboxymethyl cellulose, 0.5 parts of dibenzothiazole disulfide and 60 parts of acetic acid solution with a mass fraction of 3% are weighed and set aside;

[0063] Step S3: adding silica gel, hydrogen-terminated intermediate, nano-silicon dioxide, nano-titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 120° C. for 20 minutes, to obtain a film;

[0064] Step S4: Crush the film and place it in an oven, vulcanize it at 160°C for 15 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0065] Comparative Example 3:

[0066] This comparative example is a method for preparing a slow-rebound silica gel pillow, comprising the following steps:

[0067] Step S1: 5 g of sodium hydroxide, 25 mL of deionized water and 45 mL of anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, then 25 mmol of diethylamine is added and the temperature is raised to 50 ° C and the stirring reaction is continued for 30 min, then 10 mmol of 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 2 drops / s. After the dropwise addition is completed, the temperature is raised to 65 ° C and the stirring reaction is continued for 10 h. After the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate for 3 times, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate;

[0068] Step S2: 20 mmol 1,1,3,3-tetramethyldisiloxane, 50 mmol octamethylcyclotetrasiloxane, 70 mL and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, a gas guide tube and a reflux condenser, and nitrogen is introduced for protection. The reaction is stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 40 minutes, and then the temperature is raised to 130° C. and the stirring reaction is continued for 6 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate;

[0069] Step S3: 5.5 g of the olefin intermediate, 10 g of the terminal hydrogen intermediate, 0.03 g of chloroplatinic acid and 70 mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, and nitrogen was introduced for protection. The mixture was stirred at 30° C. and a stirring rate of 400 r / min for 30 min, and then the mixture was heated to 50° C. and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain a terminal tertiary amine intermediate;

[0070] Step S4: 70 parts of silica gel, 35 parts of terminal tertiary amine intermediate, 11 parts of nano-silicon dioxide, 9 parts of nano-titanium dioxide, 0.3 parts of sodium bicarbonate, 0.2 parts of sodium dodecyl sulfate, 3 parts of sodium carboxymethyl cellulose, 0.5 parts of dibenzothiazole disulfide and 60 parts of acetic acid solution with a mass fraction of 3% are weighed according to weight parts and set aside;

[0071] Step S5: adding silica gel, terminal tertiary amine intermediate, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stirring evenly, then adding into an open mill, mixing at a mixing temperature of 120° C. for 20 minutes, to obtain a film;

[0072] Step S6: Crush the film and place it in an oven, vulcanize it at 160°C for 15 minutes, and then melt it into a pillow mold through an extruder, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

[0073] The performance of the silica gel pillow cores in the slow-rebound silica gel pillows of Examples 1-3 and Comparative Examples 1-3 was tested, and the test results are shown in the following table:

[0074]

[0075] Referring to the data in the above table, based on the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that the slow-rebound silicone pillow of the present application has excellent antibacterial and antimicrobial properties.

[0076] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0077] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined in this application, they shall all fall within the protection scope of the present invention.

Claims

1. A slow-rebound silicone pillow, characterized in that: Includes cotton pillowcase and silicone pillow core Wherein, the silica gel pillow core comprises the following components in parts by weight: 60-70 parts of silica gel, 11-35 parts of modified silicone, 7-11 parts of nano silicon dioxide, 5-9 parts of nano titanium dioxide, 0.2-0.3 parts of sodium bicarbonate, 0.1-0.2 parts of sodium dodecyl sulfate, 1-3 parts of sodium carboxymethyl cellulose, 0.3-0.5 parts of dibenzothiazole disulfide and 40-60 parts of acetic acid solution; Wherein, the modified silicone is prepared by the following steps: Step s1: sodium hydroxide, deionized water and anhydrous ether are added to a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, and stirred for reaction for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400 r / min, then diethylamine is added and the temperature is raised to 45-50°C and the stirring reaction is continued for 20-30 minutes, then 3-bromo-1-propylene is added dropwise while stirring, and the dropping rate is controlled to be 1-2 drops / s, and after the dropwise addition is completed, the temperature is raised to 60-65°C and the stirring reaction is continued for 8-10 hours, and after the reaction is completed, the reaction product is cooled to room temperature, and then extracted with ethyl acetate 2-3 times, the extracts are combined and the solvent is removed by rotary evaporation to obtain an olefin intermediate; Step s2: 1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane and toluene are added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a reflux condenser, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 30-40 min, and then the temperature is raised to 120-130° C. and the stirring reaction is continued for 5-6 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain a terminal hydrogen intermediate; Step s3: Add the olefinic intermediate, the terminal hydrogen intermediate, chloroplatinic acid and anhydrous acetone into a three-necked flask equipped with a stirrer, a thermometer, a gas duct and a reflux condenser, introduce nitrogen protection, stir the reaction at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 min, then heat the temperature to 40-50° C. and continue stirring the reaction for 2-3 h. After the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent to obtain a terminal tertiary amine intermediate; Step s4: Add the terminal tertiary amine intermediate, monobromododecane, anhydrous potassium carbonate and anhydrous acetone into a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir the reaction at a temperature of 25-30°C and a stirring rate of 300-400r / min for 30-40min, then raise the temperature to 85-90°C and continue stirring the reaction for 15-20h. After the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent, then wash with petroleum ether and distilled water for 3-5 times in turn, then place it in a vacuum drying oven, and dry it at a temperature of 50-55°C for 3-5h to obtain modified silicone.

2. The slow-rebound silicone pillow according to claim 1, characterized in that: The usage ratio of the sodium hydroxide, deionized water, anhydrous ether, diethylamine and 3-bromo-1-propylene in step s1 is 2-5 g: 20-25 mL: 40-45 mL: 22-25 mmol: 10 mmol.

3. The slow-rebound silica gel pillow according to claim 1, characterized in that: The usage ratio of the 1,1,3,3-tetramethyldisiloxane, octamethylcyclotetrasiloxane and toluene in step s2 is 10-20 mmol:50 mmol:60-70 mL.

4. The slow-rebound silica gel pillow according to claim 1, characterized in that: The usage ratio of the alkenyl intermediate, the terminal hydrogen intermediate, chloroplatinic acid and anhydrous acetone in step s3 is 1.5-5.5 g: 10 g: 0.01-0.03 g: 60-70 mL.

5. The slow-rebound silica gel pillow according to claim 1, characterized in that: The usage ratio of the terminal tertiary amine intermediate, monobromododecane, anhydrous potassium carbonate and anhydrous acetone in step s4 is 10g:1.3-3.9g:4-6g:70-80mL.

6. A method for preparing a slow-rebound silica gel pillow, characterized in that: The following steps are involved: Step 1: Weigh 60-70 parts of silica gel, 11-35 parts of modified silicone, 7-11 parts of nano silicon dioxide, 5-9 parts of nano titanium dioxide, 0.2-0.3 parts of sodium bicarbonate, 0.1-0.2 parts of sodium dodecyl sulfate, 1-3 parts of sodium carboxymethyl cellulose, 0.3-0.5 parts of dibenzothiazole disulfide and 40-60 parts of acetic acid solution according to weight parts, and set aside; Step 2: Add silica gel, modified silicone, nano silicon dioxide, nano titanium dioxide, sodium bicarbonate, sodium dodecyl sulfate, sodium carboxymethyl cellulose, dibenzothiazole disulfide and acetic acid solution into a high-speed mixer, stir evenly, then add into an open mill, mix at a mixing temperature of 90-120° C. for 15-20 minutes to obtain a film; Step 3: Crush the film and place it in an oven, vulcanize it at a temperature of 150-160°C for 10-15 minutes, then melt it through an extruder into a pillow mold, and then solidify it to obtain a silicone pillow core, and then put the silicone pillow core into a cotton pillowcase to obtain a slow-rebound silicone pillow.

7. The method for preparing a slow-rebound silica gel pillow according to claim 6, characterized in that: The mass fraction of the acetic acid solution is 2-3%.

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