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Synthesis method of poly 6-hydroxyhexanoate

A technology of hydroxycaproic acid ester and synthesis method, which is applied in the chemical industry, can solve the problems of unstable production process and unsatisfactory yield of 6-hydroxycaproic acid ester, and achieve the effects of fast reaction progress, good production effect and simple steps

Inactive Publication Date: 2020-12-29
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, there are few technical materials and literatures on the synthesis and production of poly-6-hydroxycaproic acid ester. When our research group explored the process conditions of poly-6-hydroxycaproic acid alcoholysis reaction, depolymerization under different conditions obtained respectively Methyl 6-hydroxycaproate, ethyl 6-hydroxycaproate, propyl 6-hydroxycaproate, ethylene glycol 6-hydroxycaproate, ε-caprolactone and oligomers, of which 6-hydroxycaproic acid The yield of ethyl ester is the highest, reaching 87.006%. The yields of other 6-hydroxycaproic acid esters are all unsatisfactory, because the target product of poly6-hydroxycaproic acid alcoholysis is caprolactone, and 6-hydroxycaproic acid ester is alcohol The by-product of decomposing reaction, this is unstable as a kind of production technique of 6-hydroxycaproic acid ester, and the yield of this technique poly-6-hydroxycaproic acid ester is all more than 95%, and product component is simple and easy to separate, greatly Increased yield and productivity

Method used

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  • Synthesis method of poly 6-hydroxyhexanoate
  • Synthesis method of poly 6-hydroxyhexanoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Neutralize 30g of poly-6-hydroxycaproic acid with 0.1mol / L sodium hydroxide solution to neutrality, then add 30g of 2-chloroethanol, add DMF30g, mix and place in a 250ml round bottom flask, add at 50°C 0.3 g of tetraethylammonium bromide is placed in a collector-type constant temperature heating magnetic stirrer to obtain poly-6-hydroxycaproic acid ester through 1 h of esterification, and then add 20 ml of cyclohexane to the obtained poly-6-hydroxycaproic acid ester Alkanes were removed to obtain 32.5 g of poly-6-hydroxycaproic acid ester, and the yield of poly-6-hydroxycaproic acid ester was 98.5%.

Embodiment 2-5

[0021] The quality of poly-6-hydroxycaproic acid is the same as in Example 1, and the others are different from Example 1, see Table 1 for details.

Embodiment 6-10

[0023] The mass of poly-6-hydroxycaproic acid is 40g, and the others are different from Example 1, see Table 1 for details.

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Abstract

The invention provides a synthesis method of poly 6-hydroxyhexanoate. The method comprises the following steps: neutralizing poly 6-hydroxyhexanoic acid to be neutral by using an alkali, adding an alcohol, a catalyst and a certain amount of solvent, mixing, putting into a reactor, reacting for 1-5 h under pressure at a temperature of 50-150 DEG C, adding a water-carrying agent after the reaction is finished, and removing water by using a rotary evaporator to obtain poly 6-hydroxy hexanoate. The method has the beneficial effects that (1) the technical steps are simple, the method is simple, andthe reaction progress is fast; (2) no side reaction product is generated in the technology, other products such as salt NaCl, KBr, water and the like are easy to separate and have little influence onthe environment, and the process safety coefficient is high; and (3) the yield of the poly 6-hydroxy hexanoate is 95% or above, and the production effect is good.

Description

technical field [0001] The invention belongs to the chemical industry, in particular to a method for synthesizing poly-6-hydroxyhexanoate. Background technique [0002] Poly-6-hydroxyhexanoate is a linear polyester, very soft, has great stretchability, and has good biodegradability and biocompatibility, it can be used as a drug carrier and degradable surgical suture The production raw material can also be compatible with macromolecules such as polyethylene, polypropylene, polycarbonate, and polyvinyl chloride, and can be copolymerized to prepare a variety of copolymers or blends with excellent properties. It is a very useful organic material. However, at present, there are few technical materials and literatures on the synthesis and production of poly-6-hydroxycaproic acid ester. When our research group explored the process conditions of poly-6-hydroxycaproic acid alcoholysis reaction, depolymerization under different conditions obtained respectively Methyl 6-hydroxycaproat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/06
CPCC08G63/78C08G63/06
Inventor 谢传欣
Owner QINGDAO UNIV OF SCI & TECH
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