A kind of preparation method of lignin polyether polyol

A lignin polyether and polyol technology, applied in the field of chemical synthesis, can solve the problems of low yield of propoxylated lignin, unsuitability for industrial production, high viscosity of polyether, etc., and achieve good compatibility and stable size High performance and high mechanical compressive strength

Active Publication Date: 2018-05-04
CHINA PETROCHEMICAL CORP
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Problems solved by technology

The lignin used in this method exists in solid form, the reaction rate is slow during the reaction with epoxy compounds, the yield of propoxylated lignin is low, and the resulting polyether has high viscosity and poor compatibility with other polyethers
Document 200710131480.5 also discloses a preparation method of block polyether compound modified lignin, which is to alternately react with ethylene oxide and propylene oxide under the action of a basic catalyst to obtain a lignin block polyether compound. The method is cumbersome and not suitable for industrial production

Method used

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  • A kind of preparation method of lignin polyether polyol

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Effect test

Embodiment 1

[0039] Preparation of lignin polyether polyols:

[0040] (1) Add 200g of glycerin, 200g of sucrose and 10g of dimethylamine into the closed reaction kettle, and replace the air in the reaction kettle with nitrogen. After the temperature is raised to 100°C, slowly add 300g of propylene oxide to control the pressure inside the reaction kettle Less than 0.4MPa, due to the exothermic reaction, open the cooling water tube to cool down, and keep the temperature at 90-100°C. After adding propylene oxide, in order to completely react the propylene oxide in the gas phase in the reactor, proceed at a stirring rate of 18rpm The first section stirred and reacted for 3 hours;

[0041] (2) After reducing the pressure to 0.05MPa, degas for 1 hour;

[0042] (3) Then add 20g of sodium lignosulfonate, and slowly add the remaining 500 grams of propylene oxide, control the pressure in the reactor to be less than 0.4MPa, and the reaction temperature is 110-115°C. After adding propylene oxide, in ...

Embodiment 2

[0046] Preparation of lignin polyether polyols:

[0047] (1) Add 300 grams of glycerin and 10 grams of dimethylethanolamine into a closed reaction kettle, and replace the air in the reaction kettle with nitrogen. After the temperature is raised to 80°C, slowly add 184 g of propylene oxide to control the pressure inside the reaction kettle No more than 0.4MPa. Due to the exothermic reaction, open the cooling water tube to cool down, and control the reaction temperature at 90-100°C. After adding propylene oxide, in order to completely react the propylene oxide in the gas phase in the reactor, the stirring rate at 18rpm The next first section stirred and reacted for 2 hours;

[0048] (2) Then after the pressure drops to 0.01MPa, degas for 0.5 hours;

[0049] (3) Then add 150g of sodium lignosulfonate, and slowly add the remaining propylene oxide 736g, control the pressure in the reactor to not exceed 0.4MPa, and the reaction temperature is 100-110°C. After adding propylene oxide...

Embodiment 3

[0053] Preparation of lignin polyether polyols:

[0054] (1) Add 30g of glycerol, 60g of sucrose, 50g of sorbitol, 8g of N,N'-dimethyl 1,3 propylenediamine, and 8g of aminoethylpiperazine into the closed reaction kettle, and replace them with nitrogen After the air in the reactor is heated up to 90°C, slowly add 150g of butylene oxide to control the pressure inside the reactor to be less than 0.4MPa. Due to the exothermic reaction, open the coil to cool down the cooling water, and control the temperature at 90-100°C. After finishing the butylene oxide, in order to make the butylene oxide in the gas phase in the reactor react completely, the first section of the reaction was stirred for 2 hours at a stirring rate of 18rpm;

[0055] (2) Then the pressure drops to -0.05MPa, degassing for 0.5 hours;

[0056] (3) Then add 250g of sodium lignosulfonate, and slowly add the remaining 480g of butylene oxide, control the pressure in the reactor to be less than 0.4MPa, and the reaction ...

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Abstract

The invention relates to a preparation method of lignin polyether polyol, which is obtained by reacting lignin sulfonate and polyol as co-initiators, epoxy compound as polymerization monomer, and organic amine as catalyst. Lignin polyether polyol; the preparation method has the characteristics of low production cost, and the obtained lignin polyether polyol has good compatibility with other polyethers, and when used to prepare rigid polyurethane foam plastics, The activity is high, the mechanical compression strength of the product is higher than that of ordinary rigid foam polyether, and the cells are finer, the anisotropy is small, the dimensional stability is high, and the thermal conductivity is low, and a good technical effect has been achieved.

Description

technical field [0001] The invention relates to a preparation method of lignin polyether polyol, which belongs to the field of chemical synthesis. Background technique [0002] Lignin is the second largest type of natural aromatic polymer material after cellulose in quantity. The pulp and paper industry separates about 140 million tons of cellulose from plants every year, and at the same time obtains about 50 million tons of lignin by-products , but so far, more than 95% of lignin is still directly discharged into rivers as "black liquor" or burned after being concentrated, and is rarely used effectively, because lignin is mainly produced in the process of pulp and paper industry. The recovered by-products are very rich in resources and low in price, and will become an important resource for the preparation of polyols in the future. Lignin is a complex amorphous polymer connected by phenylpropane units of hydrophobic non-polar groups through ether bonds and carbon-carbon bo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C08G65/28C08G18/76C08G18/48C08J9/14C08G101/00
Inventor 闫鸿敏宋虹霞孙祥蒋晓群沈立飞
Owner CHINA PETROCHEMICAL CORP
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