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Preparation method of polyether polyol with high molecular weight, low unsaturation degree and high primary hydroxyl group content

A polyether polyol, high molecular weight technology, used in the chemical industry, can solve the problems of narrow molecular weight distribution, uneven molecular chain length, low viscosity, etc., and achieve the effects of short demoulding time, good physical and mechanical properties, and high activity.

Active Publication Date: 2014-10-22
SHANDONG BLUSR DONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although polyether polyols made with bimetallic catalysts (DMC) have the advantages of narrow molecular weight distribution, adjustable molecular weight, low unsaturation, and low viscosity, DMC has high catalytic activity. During the (EO) addition reaction, the chain growth rate of EO is faster than the chain transfer rate. As a result, some polyethylene oxide branch chains in the PPG finished product are very long, and some chain segments have fewer EO chains, or even no
In this way, the length of the molecular chain is uneven, the distribution of EO is uneven, and the primary hydroxyl content of the polyether is low.
Therefore, at present, when using EO end-capping to increase the number of primary hydroxyl groups, satisfactory results cannot be achieved with DMC catalysts, and alkali-based or acid-based catalysts are still required.
[0004] Usually, in the presence of a basic catalyst, EO is used to end-cap PPG to obtain terminal primary hydroxyl PPG, but this technology cannot be simply extended to the process using DMC catalyst. When EO is added to PPG containing DMC catalyst, the obtained A heterogeneous mixture of unblocked PPG, polyethylene glycol and a very small amount of high-capped PPG

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) 320g polyoxypropylene glycerol ether initiator, 0.0125g bimetallic complex catalyst, 14.4mg sulfuric acid (diluted into mass concentration is 10%) is made auxiliary agent, joins the pressure-resistant reactor of 4 liters , the contents of the reactor were vacuum dehydrated at 25° C. for 15 minutes while stirring (450 rpm) and nitrogen (50 ml / min). Vacuumize to vacuum degree -0.080Mpa, after heating up to 90°C, start nitrogen bubbling and continue heating up to 130°C, add 100g of propylene oxide to initiate. Add the remaining 2000g of propylene oxide while maintaining the temperature of the reactor at 130±3°C. After the propylene oxide is added, when the pressure of the reactor does not change, it indicates that the reaction is over, and polyether triol A is obtained. 2420g.

[0024] (2) make solvent with water, preparation mass fraction is 25% CaH 2 Aqueous solution forms a treatment agent.

[0025] (3) get the treatment agent 19.36g (CaH 2 The mass fraction of ...

Embodiment 2

[0028] (1) 125g polyoxypropylene propylene glycol ether initiator, 0.0125g bimetallic complex catalyst, 5.6mg sulfuric acid (diluted into mass concentration is 10%) is made auxiliary agent, joins in the pressure-resistant reactor of 4 liters, The contents of the reactor were vacuum dehydrated at 25° C. for 15 minutes while stirring (450 rpm) and nitrogen sparging (50 ml / min). Vacuumize to vacuum degree -0.080Mpa, after heating up to 90°C, start nitrogen bubbling and continue heating up to 130°C, add 100g of propylene oxide to initiate. Add the remaining 2000g of propylene oxide while maintaining the temperature of the reactor at 130±3°C. After the propylene oxide is added, when the pressure of the reactor does not change, it indicates that the reaction is over, and polyether diol A is obtained. 2225g.

[0029] (2) Use water as a solvent to prepare an aqueous solution of sodium carbonate with a mass fraction of 30% to form a treatment agent.

[0030] (3) Get 8.9g of the treat...

Embodiment 3

[0033] (1) 208g polyoxypropylene glycerol ether initiator, 0.0125g bimetallic complex catalyst, 9.4mg sulfuric acid (diluted into a mass concentration of 10%) is used as an auxiliary agent, and is added to a pressure-resistant reactor of 4 liters , the contents of the reactor were vacuum dehydrated at 25° C. for 15 minutes while stirring (450 rpm) and nitrogen (50 ml / min). Vacuumize to vacuum degree -0.080Mpa, after heating up to 90°C, start nitrogen bubbling and continue heating up to 130°C, add 100g of propylene oxide to initiate. Add the remaining 1892g of propylene oxide while maintaining the temperature of the reactor at 130±3°C. After the propylene oxide is added, when the pressure of the reactor does not change, it indicates that the reaction is over, and polyether triol A is obtained. 2300g.

[0034] (2) Using methanol as a solvent, prepare a methanol solution with a mass fraction of 10% tetramethylammonium hydroxide to form a treatment agent.

[0035] (3) Get 73.6g ...

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Abstract

The invention relates to a preparation method of polyether polyol with high molecular weight, low unsaturation degree and high primary hydroxyl group content, belonging to the field of chemical engineering. According to the preparation method, a treating agent is used for treating the polyether polyol with high molecular weight and low unsaturation degree, which contains bimetallic catalyst DMC; ethylene oxide is added for end capping; an adsorbent is used for treating the product of the end capping; filtration is finally carried out to obtain the polyether polyol with high molecular weight, low unsaturation degree and high activity, wherein the molecular weight of the polyether polyol is 8000-15000 and the primary hydroxyl group mole fraction is 85-93%. The prepared polyether polyol with high molecular weight, low unsaturation degree and high primary hydroxyl group content has the characteristics of high activity, short demoulding time and good physical mechanical property; by using the polyether polyol as a raw material, the prepared high-resilience moulding foam product is suitable for the preparation of various automotive trim materials. The invention expands the application of the polyether polyol to PU big high-resilience foam and one-step moulding foam.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation method of polyether polyol with high molecular weight, low unsaturation, high primary hydroxyl content and high activity. Background technique [0002] Ordinary polyether polyol (PPG) has a series of problems such as low molecular weight, high unsaturation and insufficient activity, which lead to poor product quality and application performance, which limit the application field of PPG. When the relative molecular weight of PPG is higher, the number of hydroxyl groups becomes smaller, and the relative content of primary hydroxyl groups must be increased to improve the reactivity of the product. The activity of the primary hydroxyl group is three times that of the secondary hydroxyl group. The PPG with primary hydroxyl group can shorten the curing time during foam molding. [0003] Highly active polyether prepared by traditional basic compound catalyst has high degree ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/322C08G65/324C08G65/333C08G65/331C08G65/323C08G65/328C08G65/30C08G65/26
Inventor 孙苗赵传孝秦好辉
Owner SHANDONG BLUSR DONGDA CHEM
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