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Method for preparing polyurethane heat-preserving material from epsilon-caprolactone by-product

A technology for thermal insulation materials and by-products, which is applied in the field of polyurethane thermal insulation materials prepared by the by-products of ε-caprolactone, can solve the problems of by-products in the production process of ε-caprolactone, and achieve the economic benefits of turning waste into treasure, and it is easy to obtain , the effect of solving environmental problems

Pending Publication Date: 2019-10-08
湖南东为化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention provides a method for preparing polyurethane insulation materials from ε-caprolactone by-products, which solves the problem of by-products produced in the production process of ε-caprolactone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0035] Step 1: Add 2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) In a 5L stainless steel reaction kettle, add 147.11 g of glycerin, 2.15 g of antioxidant 1010, 4.29 g of antioxidant triphenyl phosphite, and add 80 ppm of catalyst monobutyltin oxide. Raise the temperature to 140°C under stirring conditions for 1 hour, then increase the temperature at a rate of 5°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep it at 215°C for 1 hour, and measure the acid value of the system 29.36 mg KOH / g.

[0036] Add 40ppm catalyst tetrabutyl titanate, vacuumize and control the absolute vacuum to 60K Pa, and gradually increase the vacuum degree. The acid value of the system was continuously monitored during the process, and the final acid value of the system was 1.94 mg KOH / g.

[0037] Cool the reaction down to 80°C and keep it warm, spread sodium meta...

example 2

[0040] Step 1: Add 2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) In a 5L stainless steel reactor, add 154.12 g of glycerin, 2.15 g of antioxidant 1010, 4.31 g of antioxidant triphenyl phosphite, and 80 ppm of catalyst dialkyltin dimaleate. Under stirring conditions, raise the temperature to 140°C for 1 hour, then increase the temperature at a rate of 10°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep it at 220°C for 1 hour, and measure the acid value of the system 27.23 mg KOH / g.

[0041] Add 40 ppm catalyst tetrabutyl titanate, vacuumize and control the absolute vacuum to 60K Pa, and gradually increase the vacuum degree. The acid value of the system is constantly monitored during the process, and the final system acid value is below 1.83mg KOH / g.

[0042]Cool the reaction down to 80°C, spread sodium metabisulfite on the funnel (the fu...

example 3

[0045] Step 1: Add 2000.00g caprolactone by-product (acid value 128.02mg KOH / g, hydroxyl value 10.31mg KOH / g, ε-caprolactone content 17%, caprolactone oligomer 81%) In a 5L stainless steel reactor, add 145.83 g of xylitol, 2.15 g of antioxidant 1010, 4.29 g of antioxidant triphenyl phosphite, and 80 ppm of catalyst monobutyltin oxide. Raise the temperature to 140°C under stirring conditions for 1 hour, then raise the temperature at a rate of 10°C / h, and react for 1 hour at each temperature point after the temperature rise; then keep it at 215°C for 1 hour, and measure the acid value of the system 28.44 mg KOH / g.

[0046] Add 40ppm catalyst tetrabutyl titanate, vacuumize and control the absolute vacuum to 60K Pa, and gradually increase the vacuum degree. The acid value of the system was continuously monitored during the process, and the final system acid value was 1.86 mg KOH / g.

[0047] Cool the reaction down to 80°C and keep it warm, spread sodium metabisulfite on the funne...

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Abstract

The invention discloses a method for preparing a polyurethane heat-preserving material from an epsilon-caprolactone by-product. The method comprises the following steps: feeding a caprolactone by-product and micromolecular polyol in a certain proportion, adding an antioxidant and a catalyst, carrying out a reaction at 140 to 200 DEG C, then carrying out heat-preserving at 205 to 240 DEG C for 1 to3 h, adding a catalyst, and gradually reducing a pressure until an acid value of a system is no more than 2.0 mg KOH / g; subjecting a product to decolorizing treatment; and adding a foaming agent, a foam stabilizer, isocyanate and a catalyst into obtained polycaprolactone polyol, and carrying out foaming so as to prepare a polyurethane foam plastic. The polyurethane foam plastic heat-preserving material obtained by using the method provided by the invention has a heat conductivity coefficient of less than 0.10 W / (m.k) and an apparent density of less than 900 kg / m3, and can be used as a heat-preserving material. The method provided by the invention can solve the problems of recovery and utilization of a caprolactone oligomer; meanwhile, a heat-preserving material prepared by using the method provided by the invention can be used for industrial heat-preserving engineering.

Description

technical field [0001] The invention relates to a method for preparing a thermal insulation material, in particular to a method for preparing a polyurethane thermal insulation material by using ε-caprolactone by-products. Background technique [0002] ε-caprolactone (ε-CL) is an important intermediate in organic synthesis, mainly used in the synthesis of polycaprolactone polyols, polycaprolactone and other ester polymers for copolymerization and modification, because polycaprolactone Lactone has good non-toxicity, biodegradability, compatibility, and drug penetration, so it has been widely used in degradable plastics and biomedicine. [0003] The synthesis of ε-caprolactone is generally generated by Bayer-Villiger reaction of cyclohexanone, peroxyacetic acid or peroxypropionic acid under certain conditions. ε-caprolactone is a temperature-sensitive substance, which is easy to self-polymerize into oligomers with a degree of polymerization of 2-10 at high temperature. [000...

Claims

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Application Information

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IPC IPC(8): C08G18/42C08G63/08C08G63/78C08J9/12C08J9/14C08L75/06
CPCC08G18/4277C08G63/08C08G63/78C08J9/125C08J9/141C08J2203/10C08J2203/14C08J2203/182C08J2375/06
Inventor 方文拓陶丹陈卫星
Owner 湖南东为化工新材料有限公司
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