CN104650327A

CN104650327A - Poly(butylene succinate) synthesis method

Info

Publication number: CN104650327A
Application number: CN201310575746.0A
Authority: CN
Inventors: 陶建臣
Original assignee: Individual
Current assignee: Individual
Priority date: 2013-11-18
Filing date: 2013-11-18
Publication date: 2015-05-27

Abstract

The invention discloses a poly(butylene succinate) synthesis method belonging to the field of chemistry and concretely relates to poly(butylene succinate) synthesis method improvement. The poly(butylene succinate) synthesis method is simple and practical and can produce poly(butylene succinate) synthesis method with a cheap price, no toxic or side effect and recovery and recycle easiness. The poly(butylene succinate) synthesis method is characterized by comprising adding 0.10mol of succinic acid, 0.10mol of butylene glycol, a SnCl2 catalyst and 60mL of decahydronaphthalene into a four-neck flask provided with a mechanical stirrer, an oil-water separator, a nitrogen pipe and a thermometer, carrying out oil-bath heating, wherein in heating, the raw materials undergo a reaction at a temperature of 160-180 DEG C for 3h, when separated water mass is 70% of a theoretical value, the reaction product is heated to 195 DEG C so that the solution is boiling, the water enters into a water separator and the solvent flows back into the reaction system, when the total reaction time is 12.5h, stopping the reaction, cooling the reaction product to a room temperature, removing decahydronaphthalene, adding 100mL of trichloromethane into the reaction product for dissolution, carrying out filtration, carrying out deposition by 400mL of methanol under the condition of magnetic stirring to obtain white fibrous solid products and carrying out vacuum drying at a temperature of 50 DEG C for 24h.

Description

The synthetic method of poly butylene succinate

Technical field

The invention belongs to chemical field, specifically, the present invention relates to the improvement of the synthetic method of poly butylene succinate.

Background technology

Aliphatic polyester is considered to Biodegradable Materials, is the ideal substitute of conventional plastic.In aliphatic polyester family, poly butylene succinate is high with its multipolymer fusing point, has good thermoplasticity, easily processes, thus study at most.PBS and multipolymer thereof are as degradation polymer commodity selling.

Because the reaction equilibrium constant of pet reaction is low, molecular balance be reached and prepare high molecular weight product, often needing long time.Therefore, a kind of effective catalyst is found significant undoubtedly.

Summary of the invention

The present invention is exactly for above-mentioned technical problem, provides a kind of simple, practical, has no side effect, easy to be recycled, cheap poly butylene succinate synthetic method.

For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme: poly butylene succinate synthetic method of the present invention, it is characterized in that: in the four-hole bottle that mechanical stirrer, water-and-oil separator, nitrogen tube, thermometer are housed, add 0.10 mol succinic acid, 0.10 mol butyleneglycol, catalyst S nCl ₂the mol ratio of catalyzer and reactant is made to be 1/600,60 mL perhydronaphthalenes, oil bath is heated, first after 160 ~ 180 DEG C of reaction 3 h, when the quality of point water outlet reaches 70% of theoretical value, be warming up to 195 DEG C, now solution boiling, water enters water trap, solvent refluxing enters reactive system, when total reaction time reaches 12.5 h, stopped reaction, is cooled to room temperature, pour out perhydronaphthalene, after adding the dissolving of 100mL trichloromethane, filter, use 400 mL methanol extractions under magnetic stirring, obtain white fibrous solid product, at 50 DEG C of vacuum-drying 24 h.

Beneficial effect of the present invention: reaction conditions of the present invention is simple, and temperature of reaction is low, not only can produce in factory, and also easily prepare in the lab, to provide convenience condition to Product checking and experiment.

With succinic acid and butyleneglycol for raw material, take perhydronaphthalene as solvent, under catalyst action, carry out direct polymerization, synthesized high molecular weight PBS.The good catalyst of synthesis PBS, reach 79 000 with the equal relative molecular mass of PBS number that it obtains for catalyzer, productive rate reaches 9610%.When the equal relative molecular mass of number of PBS reaches more than 40 000, there is spendable mechanical property, can general-purpose plastics be replaced.The PBS synthesized by context of methods is adopted to have good biodegradability, suitable with Japanese like product, can be used as biodegradable material and use.

Embodiment

Poly butylene succinate synthetic method of the present invention, is characterized in that: in the four-hole bottle that mechanical stirrer, water-and-oil separator, nitrogen tube, thermometer are housed, add 0.10 mol succinic acid, 0.10 mol butyleneglycol, catalyst S nCl ₂the mol ratio of catalyzer and reactant is made to be 1/600,60 mL perhydronaphthalenes, oil bath is heated, first after 160 ~ 180 DEG C of reaction 3 h, when the quality of point water outlet reaches 70% of theoretical value, be warming up to 195 DEG C, now solution boiling, water enters water trap, solvent refluxing enters reactive system, when total reaction time reaches 12.5 h, stopped reaction, is cooled to room temperature, pour out perhydronaphthalene, after adding the dissolving of 100mL trichloromethane, filter, use 400 mL methanol extractions under magnetic stirring, obtain white fibrous solid product, at 50 DEG C of vacuum-drying 24 h.

Embodiment: poly butylene succinate synthetic method of the present invention, is characterized in that: add 0.10 mol succinic acid in the four-hole bottle that mechanical stirrer, water-and-oil separator, nitrogen tube, thermometer are housed, 0.10 mol butyleneglycol, catalyst S nCl ₂the mol ratio of catalyzer and reactant is made to be 1/600,60 mL perhydronaphthalenes, oil bath is heated, first after 170 DEG C of reaction 3 h, when the quality of point water outlet reaches 70% of theoretical value, be warming up to 195 DEG C, now solution boiling, water enters water trap, solvent refluxing enters reactive system, when total reaction time reaches 12.5 h, stopped reaction, is cooled to room temperature, pour out perhydronaphthalene, after adding the dissolving of 100mL trichloromethane, filter, use 400 mL methanol extractions under magnetic stirring, obtain white fibrous solid product, at 50 DEG C of vacuum-drying 24 h.

Claims

1. the synthetic method of poly butylene succinate, is characterized in that: in the four-hole bottle that mechanical stirrer, water-and-oil separator, nitrogen tube, thermometer are housed, add 0.10 mol succinic acid, 0.10 mol butyleneglycol, catalyst S nCl ₂the mol ratio of catalyzer and reactant is made to be 1/600,60 mL perhydronaphthalenes, oil bath is heated, first after 160 ~ 180 DEG C of reaction 3 h, when the quality of point water outlet reaches 70% of theoretical value, be warming up to 195 DEG C, now solution boiling, water enters water trap, solvent refluxing enters reactive system, when total reaction time reaches 12.5 h, stopped reaction, is cooled to room temperature, pour out perhydronaphthalene, after adding the dissolving of 100mL trichloromethane, filter, use 400 mL methanol extractions under magnetic stirring, obtain white fibrous solid product, at 50 DEG C of vacuum-drying 24 h.

2. the synthetic method of poly butylene succinate according to claim 1, is characterized in that: in the four-hole bottle that mechanical stirrer, water-and-oil separator, nitrogen tube, thermometer are housed, add 0.10 mol succinic acid, 0.10 mol butyleneglycol, catalyst S nCl ₂the mol ratio of catalyzer and reactant is made to be 1/600,60 mL perhydronaphthalenes, oil bath is heated, first after 170 DEG C of reaction 3 h, when the quality of point water outlet reaches 70% of theoretical value, be warming up to 195 DEG C, now solution boiling, water enters water trap, solvent refluxing enters reactive system, when total reaction time reaches 12.5 h, stopped reaction, is cooled to room temperature, pour out perhydronaphthalene, after adding the dissolving of 100mL trichloromethane, filter, use 400 mL methanol extractions under magnetic stirring, obtain white fibrous solid product, at 50 DEG C of vacuum-drying 24 h.