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A kind of preparation method of hemicellulose-based polyether polyol

A technology of polyether polyol and hemicellulose, applied in the field of organic chemical industry, can solve the problems such as no reports on the preparation of rigid foam polyether polyol from hemicellulose, achieve low shrinkage, save production costs, and avoid direct The effect of emissions

Active Publication Date: 2019-07-05
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The above studies only reported the preparation methods of polyether polyols such as sucrose, pentaerythritol, and starch; there was no report on the preparation of rigid polyether polyols from hemicellulose

Method used

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  • A kind of preparation method of hemicellulose-based polyether polyol
  • A kind of preparation method of hemicellulose-based polyether polyol
  • A kind of preparation method of hemicellulose-based polyether polyol

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Accurately weigh 60g of hemicellulose, 8.5g of potassium hydroxide, and 350g of toluene, and add them into a high-pressure reaction kettle equipped with a stirrer, a thermometer, and a circulating condenser. After nitrogen replacement, raise the temperature to 95°C, and slowly Start to feed 214g of propylene oxide, finish adding 6h, control the reaction temperature between 110-120°C, the reaction pressure is less than 0.6MPa, keep warm until the pressure no longer drops, cool down to below 60°C, and discharge; phosphoric acid is neutralized to The pH is neutral, dehydrated under reduced pressure, and filtered to obtain hemicellulose polyether polyol with a viscosity of 968mPa.s and a hydroxyl value of 368mgKOH / g, which can be used as a raw material for polyurethane rigid foam.

Embodiment 2

[0037]Accurately weigh 30g of hemicellulose, 15g of glycerin, 4g of potassium hydroxide, and 350g of toluene, and add them to a high-pressure reactor equipped with a stirrer, a thermometer, and a circulating condenser. After nitrogen replacement, raise the temperature to 95°C and stir at a constant speed. Slowly start to add 96g of propylene oxide dropwise, after 3 hours, control the reaction temperature at 130-140°C, and the reaction pressure is less than 0.6MPa, keep the temperature until the pressure no longer drops, cool down to below 60°C, and discharge; phosphoric acid is neutralized to The pH is neutral, and the hemicellulose polyether polyol is obtained by dehydration under reduced pressure and filtration. The appearance is a brownish yellow liquid, the viscosity is 3280mPa.s, and the hydroxyl value is 395mgKOH / g, which can be used as a raw material for polyurethane rigid foam.

Embodiment 3

[0039] Accurately weigh 40g of hemicellulose, 25g of glycerin, 6g of potassium hydroxide, and 350g of toluene, and add them to a high-pressure reactor equipped with a stirrer, a thermometer, and a circulating condenser. After nitrogen replacement, raise the temperature to 95°C and stir at a constant speed. Slowly start to feed 175g of propylene oxide, and finish adding in 4 hours, control the reaction temperature at 120-130°C, the reaction pressure is less than 0.6MPa, keep warm until the pressure no longer drops, cool down to below 60°C, and discharge; phosphoric acid is neutralized to pH It is neutral, dehydrated under reduced pressure and filtered to obtain hemicellulose polyether polyol, which is a brownish-yellow liquid with a viscosity of 2750mPa.s and a hydroxyl value of 390mgKOH / g, which can be used as a raw material for polyurethane rigid foam.

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Abstract

The invention discloses a preparation method of hemicellulose-based polyether polyol. The preparation method comprises the following steps: enabling hemicellulose and glycerol to be subjected to ring-opening polymerization reaction with propylene oxide under the action of a solvent and a catalyst and under the conditions that the temperature is 90 DEG C to 150 DEG C and the pressure is less than 0.6MPa, so as to prepare the hemicellulose-based polyether polyol. The solvent is selected from dimethylformamide, toluene and dioxane; the catalyst is selected from potassium hydroxide, potassium methoxide, potassium hydroxide and sodium methoxide; the mass ratio of raw materials is that the ratio of m(propylene oxide) to m(hemicellulose) to m(glycerol) is (5 to 10) : 2 : (0 to 1); the mass dosage of the solvent is 3 to 8 times that of the hemicellulose and the dosage of the catalyst is 2 percent to 8 percent of the mass of the hemicellulose. According to the method disclosed by the invention, the polyhydroxy hemicellulose recycled from viscose fiber wastewater is used as the raw material for preparing the hemicellulose-based polyether polyol and the hemicellulose-based polyether polyol can be used for preparing rigid polyurethane foam, so that waste resources can be effectively and reasonably utilized and the environment pressure is alleviated; the utilization rate of the waste resources is high and the cost is low, so that the practicability is very good.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a method for preparing hemicellulose polyether and rigid polyurethane foam by using hemicellulose recovered from viscose fiber waste water, in particular to a hemicellulose-based polyether polyol Preparation. Background technique [0002] Viscose fiber is made of mixed wood pulp of coniferous leaves and broad leaves, and is made into soluble cellulose sulfonate through alkalization, aging, sulfonation and other processes, and then dissolved in dilute lye to make viscose, which is wet-spun In the production process, a large amount of alkaline wastewater containing hemicellulose is produced, and it is directly used as wastewater for biochemical treatment, which is not only technically difficult, wastes resources, but also pollutes the environment and poses a threat to human health; how to treat the above-mentioned organic Effective comprehensive utilization of hemi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G18/48
CPCC08G18/48C08G65/2609C08G2110/0025
Inventor 朱新宝韦娴戴荪尹佳伟邓传东张金慧陈慕华余奇伟李雪梅高超锋龙国强
Owner NANJING FORESTRY UNIV
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