PBS household degradable floss pick and preparation method thereof
By combining modified polybutylene succinate material and UHMWPE, the problems of non-degradability and poor fluidity of traditional floss rod materials were solved, and PBS household floss rods with high mechanical properties and excellent degradability were prepared to achieve Environmentally friendly floss rod production.
Patent Information
- Application Number
- CN202411269529.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-11
- Publication Date
- 2024-12-13
AI Technical Summary
Traditional floss rod materials are non-degradable, resulting in environmental pollution. The existing biodegradable materials are poor in fluidity and are prone to deformation during injection molding, making them difficult to widely use.
Using modified polybutylene succinate material and UHMWPE material, high molecular weight polybutylene succinate is prepared through titanium-silicon molecular sieve, esterification and polycondensation reaction, and PBS household degradable floss is prepared in combination with high-speed injection molding technology. Great.
The prepared floss rod has excellent mechanical properties and biodegradability. It completely degrades under the action of natural microorganisms, reduces environmental load, and has a weight loss rate of up to 99.82-99.96%.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of dental floss stick production, and in particular to a PBS household degradable dental floss stick and a preparation method thereof. Background Art
[0002] Traditional dental floss stick handles are made of non-degradable materials such as polypropylene (PP) and polystyrene (PS) by injection molding. Since dental floss sticks are disposable products and are consumed in large quantities, such non-degradable materials will cause serious environmental pollution. In the prior art, there is a polyester polymer obtained by polymerization with lactic acid as the main raw material. It is a commonly used biodegradable material that can be completely degraded into carbon dioxide and water. Applying this biodegradable material to the production of dental floss sticks can effectively alleviate environmental pressure. However, this material also has certain defects. When the dental floss stick body is injection molded, it has poor fluidity and is not easy to mold. At the same time, the final formed dental floss stick body is easy to deform.
[0003] Polybutylene succinate (PBS) is an aliphatic polyester. It has the advantages of soft molecular chain, good transparency, high gloss, strong heat resistance and good processability, so it can be widely used in cold and hot beverage packaging and lunch boxes. PBS entered the field of material research in the 1990s and quickly became one of the hot materials in the research of general biodegradable plastics that are widely promoted and applied. PBS will only degrade under the conditions of contact with specific microorganisms such as compost and water. Its performance is very stable during normal storage and use, and it has good application prospects. Summary of the invention
[0004] In order to solve the above technical problems, the present invention provides a PBS household degradable dental floss stick and a preparation method thereof.
[0005] The purpose of the present invention can be achieved through the following technical solutions: A PBS household biodegradable dental floss stick, comprising a dental floss stick body, a dental floss head arranged at one end of the dental floss stick body, and a toothpick head arranged at the other end of the dental floss stick; the dental floss stick body is made of modified polybutylene succinate material, and the dental floss is made of UHMWPE material; The modified polybutylene succinate material is prepared by the following steps: 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O)The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: Succinic acid, succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached more than 90% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. Further, the mass ratio of succinic acid to succinic anhydride is 26.3-52.7:22.3-44.7; 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material.
[0006] A method for preparing a PBS household degradable dental floss stick comprises the following steps: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material is heated to 160-200° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss through an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained.
[0007] Beneficial effects of the present invention: The household dental floss stick prepared by the present invention uses a synthesized high molecular weight polybutylene succinate material as the main material of the dental floss stick, and not only has excellent mechanical properties and heat resistance, but also has biodegradability, does not increase the load on the environment, and can be degraded by the action of microorganisms existing in nature in soil, sand, composting, anaerobic digestion or aqueous culture medium, and finally completely degraded into carbon dioxide, methane, water and mineralized inorganic salts of the elements contained therein. DETAILED DESCRIPTION
[0008] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. 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. Example 1
[0009] The modified polybutylene succinate material is prepared by the following steps: 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O) The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: 52.7 g of succinic acid, 22.3 g of succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached 92% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material. Example 2
[0010] 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O)The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: 39.5 g of succinic acid, 33.5 g of succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached 93% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material. Example 3
[0011] 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O) The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: 31.6 g of succinic acid, 40.2 g of succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached 95% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material. Example 4
[0012] 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O) The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: 26.3 g of succinic acid, 44.7 g of succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached more than 90% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material. Example 5
[0013] A method for preparing a PBS household degradable dental floss stick comprises the following steps: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material prepared in Example 1 is heated to 160° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss by an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained. Example 6
[0014] A method for preparing a PBS household degradable dental floss stick comprises the following steps: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material prepared in Example 2 is heated to 170° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss by an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained. Example 7
[0015] A method for preparing a PBS household degradable dental floss stick comprises the following steps: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material prepared in Example 3 is heated to 190° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss by an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained. Example 8
[0016] A method for preparing a PBS household degradable dental floss stick comprises the following steps: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material prepared in Example 4 is heated to 200° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss by an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained.
[0017] Comparative Example Commercially available dental floss picks (Mother Deer).
[0018] The dental floss sticks of Examples 5-8 and the comparative example were subjected to degradation tests. The dental floss sticks were placed in a soil environment with a temperature of 25°C and a humidity of 60°C and containing bacteria and other microorganisms, and then taken out after being buried for 100 days to calculate the weight loss rate. The test results are shown in the following table:
[0019] It can be seen from the above table that the weight loss rate of the dental floss stick prepared by the present invention is 99.82-99.96%, and has excellent degradability.
[0020] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field 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 scope defined by the concept of the invention, they should all fall within the protection scope of the present invention.
Claims
1. A PBS household biodegradable dental floss stick, characterized in that: The structure comprises a dental floss stick body, a dental floss head arranged at one end of the dental floss stick body, and a toothpick head arranged at the other end of the dental floss stick; the dental floss stick body is made of modified polybutylene succinate material, and the dental floss is made of UHMWPE material; The modified polybutylene succinate material is prepared by the following steps: 1) Preparation of titanium silicate molecular sieve: 3.4g Ti(OC4H9)4, 64.5g TEOS, 16.27g TPAOH and 90mL deionized water, molecular weight n (TiO2) :n (SiO2) :n (TPAOH) :n (H2O) The mixture is 1:30:8:500, mixed evenly, placed at 35°C for reaction for 3 hours, then added into a kettle with a polytetrafluoroethylene liner, crystallized at 140°C for 1 hour to obtain a directing agent; Then, 1 g of CTAB, 20 mL of 25 wt% ammonia water, 100 mL of deionized water and 1 g of directing agent were mixed evenly, reacted at 30° C. for 5 h, added into a kettle lined with polytetrafluoroethylene and crystallized at 120° C. for 12 h, and the obtained product was filtered, washed, dried at room temperature, and calcined at 500° C. for 4 h to obtain titanium silicalite molecular sieve; 2) Esterification reaction: Succinic acid, succinic anhydride and 72.1 g of 1,4-butanediol were added to a 200 mL reactor. The reaction was carried out under normal pressure. The reaction started when the first drop of water was distilled out. The amount of water produced was recorded every 30 minutes. During the reaction, the temperature in the reactor was controlled at 150°C. When the amount of water produced reached more than 90% of the theoretical calculated value of the esterification rate, the reaction was stopped. After cooling, the esterification product was obtained. 3) Polycondensation reaction: Add 50g of the esterification product to a reactor equipped with a stirring device, heat it to 120°C, then add 0.5g of titanium silicon molecular sieve, continue to heat it to 220°C, and then evacuate to about 50Pa. After reacting for 2.5h, cool it down, add anhydrous ethanol to wash, filter, and then dry it in a vacuum drying oven at 80°C for 24h to obtain the modified polybutylene succinate material.
2. A PBS household degradable dental floss stick according to claim 1, characterized in that: The mass ratio of succinic acid to succinic anhydride in the esterification reaction is 26.3-52.7:22.3-44.
7.
3. The method for preparing a PBS household degradable dental floss stick according to claim 1, characterized in that: The following steps are involved: The dental floss made of UHMWPE material is placed in a mold for making a dental floss stick. The modified polybutylene succinate material is heated to 160-200° C. by a heating device using a high-speed injection molding machine. The heated plastic material is then injected into the mold containing the dental floss through an injection device. After naturally cooling to room temperature, a PBS household biodegradable dental floss stick is obtained.