1,3-propanediol and preparation method thereof

A technology for esterification and reactant, which is applied in the field of solid esterification and its melt condensation preparation based on the difference in the reactivity of the multifunctional groups of the reactants, can solve the problems of environmental pollution in the preparation process, difficulty in storage and use, and low content of functional elements, etc. Achieve the effect of overcoming easy migration, beneficial to environmental protection and simple method

Active Publication Date: 2017-06-20
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of traditional liquid esters such as difficulty in storage and use, pollution of the environment during the preparation process, low content of functional elements, and low molecular weight, and to prepare a product with less pollution in the preparation process, high content of functional elements and low molecular weight. high solid ester

Method used

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  • 1,3-propanediol and preparation method thereof
  • 1,3-propanediol and preparation method thereof
  • 1,3-propanediol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0044] A kind of preparation method of esterification compound, the steps are as follows:

[0045] 1) The side group phosphorus-containing dibasic acid [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)methyl]succinic acid (DDP ) and pentaerythritol are mixed with a molar ratio of 4:1, under the conditions of inert gas nitrogen protection and mechanical stirring, the melt esterification reaction is carried out, the stirring speed of the mechanical stirrer is 300rpm, the temperature of the melt esterification reaction is 180 ℃, and the reaction time is After 1h, the product was collected after the reaction, dissolved, filtered and dried to obtain DAPER whose end group was carboxyl; the reaction equation is as follows:

[0046]

[0047] 2) Mix phenylphosphonic acid and glycol with a molar ratio of 1:1, add catalyst 4-methylbenzenesulfonic acid, the molar ratio of phenylphosphonic acid and catalyst is 1:0.01, under inert gas nitrogen protection and The melt condensation reaction...

Embodiment 4～6

[0057] A kind of preparation method of esterification compound, the steps are as follows:

[0058] 1) Mix side group nitrogen-containing dibasic acid and pentaerythritol in a molar ratio of 4:1, and carry out melt esterification reaction under the conditions of inert gas nitrogen protection and mechanical stirring, the stirring speed of mechanical stirring is 310rpm, melt esterification reaction The temperature is 180°C, and the reaction time is 2 hours. After the reaction, the product is collected, dissolved, filtered and dried to obtain DAPER whose end group is a carboxyl group; the reaction equation is as follows:

[0059]

[0060] 2) Mix phenylphosphonic acid and glycol with a molar ratio of 1:2, add catalyst 4-methylbenzenesulfonic acid, the molar ratio of phenylphosphonic acid and catalyst is 1:0.01, under inert gas nitrogen protection and The melt condensation reaction was carried out under the condition of mechanical stirring, the stirring speed of the mechanical st...

Embodiment 7～9

[0071] A kind of preparation method of esterification compound, the steps are as follows:

[0072] 1) Mix side group nitrogen-containing dibasic acid and pentaerythritol in a molar ratio of 4:1, and carry out melt esterification reaction under the conditions of inert gas nitrogen protection and mechanical stirring. The stirring speed of mechanical stirring is 340rpm, and melt esterification reaction The temperature is 182°C, and the reaction time is 3 hours. After the reaction, the product is collected, dissolved, filtered and dried to obtain DAPER whose terminal group is a carboxyl group; the reaction equation is as follows:

[0073]

[0074] 2) Methylphosphonic acid and dibasic alcohol are mixed with the molar ratio of 1:1, add catalyst 4-methylbenzenesulfonic acid, the molar ratio of methylphosphonic acid and catalyst is 1:0.01, under inert gas nitrogen protection and The melt condensation reaction is carried out under the condition of mechanical stirring, the stirring s...

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Abstract

The invention relates to 1,3-propanediol and a preparation method thereof. Firstly, through the melt esterification reaction between dibasic acid and pentaerythritol, DAPER with the terminal group being carboxyl is prepared; then, DADA with the terminal group containing carboxyl is prepared through the melt condensation reaction between the double-functional-group organic acid containing functional elements and dihydric alcohol; the double functional groups in the double-functional-group organic acid containing functional elements are selected from phosphate, carboxylic group and hydrosulphonyl; the functional elements are one kind of materials from P, S and N, or the combination of S and N; finally, the DAPER is added into the DADA to prepare the final product through the esterification reaction between the DAPER and the DADA. The defects of storage and use difficulty, single purpose due to simple structure, environment pollution in the preparation process and the like of the conventional liquid type 1,3-propanediol are overcome. The finally prepared 1,3-propanediol is solid materials with the high molecular weight; the terminal group of the molecule is a reaction active group; 8.14 to 18.32 weight percent of functional elements are contained inside the terminal group of the molecule; the advantages of high thermal stability, wide purposes and the like are realized.

Description

technical field [0001] The invention belongs to the field of flame retardants, and relates to an esterified product and a preparation method thereof, in particular to a solid esterified product and its melt condensation preparation method based on the difference in reactivity of reactant multifunctional groups. Background technique [0002] With the development of my country's synthetic material industry and the continuous expansion of application fields, it has been widely used in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, basic necessities of life, etc. But most of them are flammable materials, which are easy to cause fire and pose a great threat to life and property safety. Therefore, the flame retardancy of polymer materials has become an urgent problem to be solved. At present, various types of polymers are widely used to add flame retardants to improve the flame retardancy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C07F9/58C07F9/6503C07F9/6506C07D401/14C07D233/56C08K5/5313C08K5/5357C08K5/5373C08K5/3445
CPCC07D233/56C07D401/14C07F9/58C07F9/65031C07F9/6506C07F9/657172C08K5/3445C08K5/5313C08K5/5357C08K5/5373
Inventor 孙宾朱美芳计虎泉江晓泽相恒学滕伟
Owner DONGHUA UNIV
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