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Preparation method of modified polyester polyol

A technology of polyester polyol and modified polyester, which is applied in the field of polymer compound preparation, can solve the problems of long unit operation time, unfavorable biological utilization, easy oxidation and blackening, etc., and achieves operation time saving, novel catalyst and coloring low degree of effect

Inactive Publication Date: 2018-09-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] CN101168592A discloses a polyester polyol and its preparation method and application. The patented three-step method for preparing caprolactone-modified polyester polyol requires multiple operations of heating, cooling, and feeding. The steps are cumbersome and the unit operation time is Long, using transition metal compounds such as tin and pickaxe as catalysts, transition metal catalysts are easy to oxidize and blacken, causing material discoloration, and at the same time, transition metal catalysts have certain toxicity, which is not conducive to biological utilization

Method used

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  • Preparation method of modified polyester polyol
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Examples

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Embodiment 1

[0034] 1M of P 4 -t-Bu (1mL), polyethylene adipate (10.02g, 10mmol) with a molecular weight of about 1000g / mol and toluene (30mL) are prepared into solution A in an 80mL ampoule by Schlenck technology; the solution will be passed through GaH 2 In addition to water, the monomer ε-caprolactone (11.41g, 100mmol) and toluene (30mL) after distillation under reduced pressure were prepared into solution B in an 80mL ampoule via schlenk technology; solution A and solution B were transferred via schlenk technology respectively Into two 50mL airtight syringes; press solution A and solution B into the T / Y mixer at the same flow rate; react in a reaction coil (VL=2mL) with an inner diameter of 1.0 mm at 20°C, The effluent was collected with methanol and quenched with benzoic acid. The flow rate is adjusted to 0.1mL / min, the reaction time is 10min, the conversion rate of ε-caprolactone is 98.36%, the molecular weight can reach 2000g / mol, the PDI value is 1.08, the water content is ≤0.1%, and...

Embodiment 2

[0036] 1M of P 4 ---t-Oct (1mL), polybutylenemalonate (1.19g, 1mmol) and chloroform (30mL) with a molecular weight of about 1200g / mol are formulated into solution A in an 80mL ampoule via schlenck technology; The monomer trimethylene carbonate (3.67g, 30mmol) and chloroform (30mL) were recrystallized and purified from ethyl acetate to prepare solution B in an 80mL ampoule by Schlenk technology; solution A and solution B were passed through The schlenk technology was transferred to two 50mL air-tight syringes; solution A and solution B were pressed into the T / Y mixer at the same flow rate; at 30℃, the reaction coil with an inner diameter of 1.0mm (VL=2mL) The reaction was stopped, the effluent was collected with methanol and quenched with benzoic acid. The flow rate is adjusted to 66.67μL / min, the reaction time is 15min, the trimethylene carbonate conversion rate reaches 99.12%, the molecular weight can reach 4200g / mol, the PDI value is 1.06, the water content is ≤0.1%, and the ...

Embodiment 3

[0038] 1M of P 4 -t-Bu (1mL), a molecular weight of about 1500g / mol polypropylene glycol (1.52g, 1mmol) and dichloromethane (30mL) are prepared into solution A in an 80mL ampoule by Schlenck technology; it will be passed through ethyl acetate The monomer lactide (7.21g, 50mmol) and dichloromethane (30mL) purified by medium recrystallization were formulated into solution B in an 80mL ampoule by schlenk technology; solution A and solution B were transferred to two by schlenk technology. In a 50mL airtight syringe; press solution A and solution B into the T / Y mixer at the same flow rate; react in a reaction coil (VL=2mL) with an inner diameter of 1.0 mm at 25°C, and discharge the liquid Collect with methanol and quench with benzoic acid. The flow rate is adjusted to 50μL / min, the reaction time is 20min, the lactide conversion rate reaches 99.57%, the molecular weight can reach 8500g / mol, the PDI value is 1.07, the water content is ≤0.1%, and the color (APHA) value is 22.

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Abstract

The invention discloses a preparation method of modified polyester polyol. The method comprises the following steps that cyclic ester is used as a monomer; polyester polyol is used as a macromoleculeinitiating agent; a microchannel reaction device is used as a reactor; under the existence of catalysts and reaction solvents, chain extension reaction is performed to obtain the modified polyester polyol. A micro-reaction device is used; the continuous production is realized; the operation time is saved; the operation steps are simplified; the reaction time is shortened; the reaction conditions are mild.

Description

Technical field [0001] The invention relates to a method for preparing a polymer compound, in particular to a method for preparing a modified polyester polyol. Background technique [0002] Polyester polyol is one of the important raw materials for the synthesis of polyurethane (PU), and acts as a soft soft segment in the synthesis of polyurethane. The polyester polyol required in polyurethane has a relatively low molecular weight, generally 1000 to 3000 g / mol. Polyester polyols are usually linear polymers prepared by polycondensation of dibasic acids and dihydric alcohols. The polycondensation reaction is a reversible reaction. As the viscosity of the system increases in the later stage of the reaction, the generated water is not easily discharged from the system. Measures such as increasing the temperature, increasing the stirring rate and applying vacuum are required to maintain the reaction in a positive direction. However, if the reaction time at this stage is too long, it...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/87C08G63/78
CPCC08G63/785C08G63/87C08G63/916
Inventor 郭凯高晗朱宁胡欣方正段金电邱江凯
Owner NANJING UNIV OF TECH
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