Formula and preparation method of enzymatic hydrolysis (EH) lignin modified polyalcohol

A technology for enzymatic hydrolysis of lignin and polyol, applied in the field of polymer material preparation, can solve the problems of difficulty in dissolving, affecting the promotion and application of lignin, poor solubility of enzymatic lignin, etc., and achieves low manufacturing cost, high purity, and high retention. effect of chemical activity

Inactive Publication Date: 2012-07-04
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to its own structure, the solubility of enzymatic lignin is poor. It is difficult to dissolve when using enzymatic lignin to replace some polyols to prepare polyurethane and alkyd resin, forming a homogeneous system, which directly affects the promotion and application of lignin.

Method used

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  • Formula and preparation method of enzymatic hydrolysis (EH) lignin modified polyalcohol
  • Formula and preparation method of enzymatic hydrolysis (EH) lignin modified polyalcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Example 1: Preparation of modified polyol with polyethylene glycol as the main liquefaction reagent

[0058] .Take 80g polyethylene glycol-400, 25g glycerol, 2.5g concentrated sulfuric acid, mix these three components evenly, put them in a three-necked flask and preheat to 45℃, add 25g enzymatic lignin under stirring, Warm up to 170℃, react for about 1h under the protection of nitrogen, then terminate, adjust to neutral with 5% sodium hydroxide solution, after cooling, the product is passed through a dialysis membrane to remove inorganic salts, that is, dark red liquid-like enzymatic lignin modification Polyol is about 126g. The obtained product has a hydroxyl value of 384mgKOH / g and a viscosity of 2270mPa·s. The product has a high hydroxyl value and is a uniform liquid, which can directly react with cyanate esters to synthesize polyurethane and solve the problem of insoluble and insoluble lignin. , Affecting the preparation of lignin-modified polyurethane.

Embodiment 2

[0059] Example 2: Preparation of modified polyol with polyethylene glycol as the main liquefaction reagent

[0060] Take 80g polyethylene glycol-600, 20g glycerol, 1.2g concentrated sulfuric acid and 1.8g glacial acetic acid, mix these three components uniformly, put them in a three-necked flask and preheat to 45℃, add 20g enzyme under stirring Dissolve lignin, heat up to 130°C, react for about 1h under nitrogen protection, then terminate, adjust to neutral with 5% sodium hydroxide solution, after cooling, the product is passed through a dialysis membrane to remove inorganic salts to obtain dark red liquid enzymatic hydrolysis The lignin modified polyol is about 118g. The obtained product has a hydroxyl value of 322mgKOH / g and a viscosity of 5130mPa·s. The product has a high hydroxyl value and is a uniform liquid, which can directly react with cyanate esters to synthesize polyurethane and solve the problem of insoluble and insoluble lignin. , Affecting the preparation of lignin...

Embodiment 3

[0061] Example 3: Preparation of modified polyol with mixture of polyethylene glycol and polypropylene glycol as main liquefaction reagent

[0062] Take 45g polyethylene glycol-400, 45g polypropylene glycol-400, 6g glycerol, 2.0g glacial acetic acid and 0.5g concentrated nitric acid, mix these five components uniformly, place them in a three-necked flask and preheat to 45℃ Add 15g of enzymatic lignin under stirring, heat up to 150℃, and terminate the reaction under nitrogen protection for 1 hour. Use a 28% ammonia solution to adjust to neutrality. After cooling, the product is passed through a dialysis membrane to remove inorganic salts. 114g of red liquid enzymatic hydrolysis of lignin-modified polyol. The obtained product has a hydroxyl value of 227mgKOH / g and a viscosity of 530mPa·s. The product has a high hydroxyl value and is a uniform liquid, which can directly react with cyanate esters to synthesize polyurethane. It solves the problem of insoluble and insoluble lignin. ,...

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Abstract

The invention provides a formula and a preparation method of enzymatic hydrolysis (EH) lignin modified polyalcohol. The formula comprises the following components in parts by weight: 8-50 parts of EH lignin, 50-80 parts of polyalcohol, 5-25 parts of glycerol, 1-7 parts of acid catalyst and 1-8 parts of alkali regulator. The preparation method comprises the following the steps: evenly mixing the polyalcohol, the glycerol and the acid catalyst according to the blending ratio, and preheating to the temperature of 40-55 DEG C; adding the EH lignin while stirring, boosting the temperature to 100-180 DEG C, and reacting for 1.0-4.0h under the protection of inert gas; and adding the alkali regulator so as to regulate the pH value of the solution to be 7.0-7.5, dialyzing, and performing reduced pressure distillation to obtain the enzymatic hydrolysis (EH) lignin modified polyalcohol which can be directly used for synthesizing polyurethane. The invention prepares reproducible biological resource EH lignin into liquid polyalcohol, solves the defects that the EH lignin has poor dissolubility and is difficult to be used as a modifier for the polyurethane and alkyd resin, can replace part of petrochemical complex raw materials, and lowers the production cost of the polyalcohol; and the enzymatic hydrolysis (EH) lignin modified polyalcohol has good application effect, simple process and easy implementation.

Description

technical field [0001] The invention belongs to the field of polymer material preparation, and more specifically relates to a raw material formula and a preparation method of enzymolysis lignin modified polyol. Background technique [0002] With the deepening of human understanding of environmental pollution and resource crisis, the renewable and degradable properties of natural polymers have attracted increasing attention. Recycling of waste is a major issue in contemporary economic and social development, and it is also a new requirement for contemporary science and technology. [0003] Polyol is one of the main raw materials for synthesizing polyurethane resin or alkyd resin. Polyurethane and alkyd resins have a variety of properties and uses, and have excellent properties such as wear resistance, oil resistance, chemical corrosion resistance, and radiation resistance. They are widely used in the fields of fibers, elastomers, coatings, soft and hard foam plastics, and ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C08G18/64C08G63/66C08G63/49
Inventor 程贤甦靳艳巧
Owner FUZHOU UNIV
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