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A block copolyester, biological technology, applied in the field of preparation of biodegradable block copolyester, can solve the problems of low melting point, poor strength, etc., and achieve the effect of good mechanical properties, simple and fast method, and convenient method
Inactive Publication Date: 2009-07-08
TONGJI UNIV
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[0003] Polybutylene adipate (PBA) is a degradable aliphatic polyester with several methylene groups connected in the molecular chain, so it has good flexibility, but poor strength and low melting point
Method used
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Embodiment 1
[0026] Add 1.0 moles of adipic acid, 1.2 moles of 1,4-butanediol, and 0.4384 g of tetrabutyl titanate into the reaction kettle, stir and mix evenly, and then raise the temperature to 170°C under the protection of nitrogen , maintain this temperature and react for 3.5 hours at a stirring speed of 80r / min, then reduce the pressure in the kettle to 0.4MPa, and the reaction temperature is 175 degrees. Butylene adipate prepolymer.
[0027] Add 0.8 moles of butanediol terephthalate, 1.2 moles of 1,4-butanediol, and 0.3884 g of tetrabutyl titanate into the reaction kettle, stir and mix evenly, and then, under the protection of nitrogen, , heated up to 150°C, kept at this temperature and reacted at normal pressure for 4 hours at a stirring speed of 80r / min, then stopped the reaction and discharged, to obtain a low molecular weight polybutylene terephthalate prepolymer.
[0028] Add 1.0 mol of polybutylene adipate prepared above, 0.8 mol of polybutylene terephthalate, and 0.2987 g of ...
Embodiment 2
[0031] Based on Example 1, the addition amount of 1,4-butanediol in the esterification reaction stage of step (1) is 1.3mol, and the addition amount of tetrabutyl titanate is 0.5115g; step (2) transesterification reaction stage 1 , the added amount of 4-butanediol was 1.4 mol, and the added amount of tetrabutyl titanate was 0.4661 g. Other reaction conditions and operation are identical with embodiment 1, obtain product at last.
[0032] After testing, the intrinsic viscosity of the product is 1.1839dl / g, the melting point is 132°C, the tensile strength is 29MPa, the elongation at break is 1023%, L BA =3.17,L BT = 3.58, R = 0.59.
Embodiment 3
[0034] Based on Example 1, the reaction temperature of the esterification reaction stage of step (1) is changed to 180° C., and the reaction temperature of the transesterification reaction stage of step (2) is changed to 160° C., and other reaction conditions and operations are the same as in Example 1.
[0035] After testing, the intrinsic viscosity of the product is 1.2617dl / g, the melting point is 133°C, the tensile strength is 33MPa, the elongation at break is 1096%, L BA =3.71, L BT = 3.85, R = 0.53.
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Abstract
The invention belongs to the technical field of macromolecular materials, and in particular relates to a preparation method for biodegradable blocked copolyester. The preparation method comprises the following steps: carrying out esterification reaction between adipate and 1,4 butanediol in the presence of catalyst, wherein the reaction time is 3 to 5h, nitrogen is adopted for protection, the reaction pressure is between 0.1 and 0.8MPa and the reaction temperature is between 130 and 180 DEG C during a first stage; and the reaction time is 1.5 to 5h, the reaction pressure is between 0.3 and 0.6MPa and the reaction temperature is between 150 and 200 DEG C during a second stage so as to generate polybutylene adipate; and carrying out ester exchange reaction of dimethyl terephthalate (DMT) and 1,4 butanediol in the presence of catalyst, wherein the nitrogen is adopted for protection, the reaction time is 2 to 5h, the reaction pressure is between 0.1 and 0.7MPa and the reaction temperature is between 150 and 170 DEG C so as to generate polybutylene terephthalate (pbt); and mixing both prepolymers and carrying out melt copolycondensation reaction under negative pressure, wherein the vacuum degree is controlled to be between 0 and 200Pa, the reaction temperature is between 210 and 260 DEG C and the reaction time is 3 to 8h. The preparation method carries out esterification reaction and ester exchange reaction, and the esterification reaction has two stages so as to effectively reduce secondary reaction of 1,4 butanediol. A prepared product has a characteristic viscosity number above 1.2dl/g, a melting point controlled between 100 and 140 DEG C, a tensile strength between 18 and 37MPa and a breaking elongation ratio from 800 to 1,500 percent.
Description
technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a biodegradable block copolyester. Background technique [0002] Due to its low melting point and poor mechanical properties, it is difficult for aliphatic polyester to meet the various requirements for material properties in the actual application process. At the same time, the cost of raw materials is high and the price of products remains high, which has become a bottleneck restricting its further development. Thermoplastic aromatic polyester has stable thermal properties, excellent mechanical properties, easy processing, and low price, but its biodegradability is poor, so it cannot be used alone as a degradable material. Therefore, the preparation of aliphatic-aromatic copolyesters with both the degradability of aliphatic polyesters and the excellent mechanical and thermal properties of aromatic polyesters has broad development pr...
Claims
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Application Information
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