Preparation method for block oligomeric dihydric alcohol with controllable structure

A technology of polyglycol and glycol, which is applied in the field of preparation of block-type oligomer glycol, can solve the problem of inability to synthesize segment block-type oligomer glycol and the like, and achieves a double metal cyanide catalyst. The effect of low concentration, low viscosity and moderate price

Active Publication Date: 2014-07-09
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention provides a block-type oligomeric diol with a controllable structure and a preparation method thereof, which solves the problem in the prior art that a block-type oligomeric diol with a long chain segment and a controllable structure cannot be synthesized

Method used

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  • Preparation method for block oligomeric dihydric alcohol with controllable structure
  • Preparation method for block oligomeric dihydric alcohol with controllable structure
  • Preparation method for block oligomeric dihydric alcohol with controllable structure

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preparation example Construction

[0040] The preparation method of polycarbonate diol is as follows:

[0041] Carbonic acid ester and dibasic alcohol are metered and thrown in the reaction kettle according to the ratio in the following table 1 according to a certain molar ratio, then add tetrabutyl titanate whose consumption is 0.25wt% of the dibasic alcohol feeding amount, pass into N 2 To exclude the air in the reaction system, heat the reaction system under normal pressure to gradually increase the temperature of the reaction system to 120° C., and react for 2 hours. Then gradually increase the temperature of the reaction system to 160°C, and react for 6 hours; finally, raise the temperature of the system to 180°C, then gradually reduce the absolute pressure of the system to 8kPa, keep the absolute pressure at 8KPa for 4h, and then cool to obtain a certain relative molecular mass. polycarbonate diol (PCDL).

[0042] Table 1 material ratio

[0043]

[0044] Polyester polyol:

[0045] 7. Polybutylene ad...

Embodiment 1

[0052] Embodiment 1: the preparation of a kind of block type oligomeric glycol, its preparation method is:

[0053] (1) Add 200g of polycarbonate diol PCDL-1 and 0.0123g of double metal cyanide complex catalyst DMC-B into a pressure-resistant stainless steel reactor with a volume of 1L, replace the air with nitrogen twice, start stirring, and heat to 110°C, remove moisture in vacuum for 1h.

[0054] (2) Then heat up to 120°C, first add 53g of propylene oxide to the reaction kettle in the above (1) for induction reaction, after the induction reaction is completed, gradually add the remaining 158g of propylene oxide dropwise, after the reaction is completed, remove Unreacted propylene oxide, to obtain block-type oligomeric diols, the yield is 99.2%, and the hydroxyl value measured by the phthalic anhydride-pyridine method (GB / T12008.3-2009) is 56.8mg KOH / g, and the average molecular weight is 1975.

[0055] The product structure formula is:

[0056]

Embodiment 2

[0062] Embodiment 2: the preparation of a kind of block type oligomeric glycol, its preparation method is:

[0063] (1) Add 200g of polycarbonate diol PCDL-2 and 0.628g of double metal cyanide complex catalyst DMC-A into a pressure-resistant stainless steel reactor with a volume of 1L, replace the air with nitrogen for 3 times, start stirring, and heat to 120°C, remove moisture under vacuum for 1h.

[0064] (2) Then heat up to 130°C, first add 128g propylene oxide to the reaction kettle in the above (1) for induction reaction, after the induction reaction is completed, gradually add the remaining 300g propylene oxide dropwise, after the reaction is completed, remove Unreacted propylene oxide, obtain block type oligomeric diol, yield is 98.8%, measure hydroxyl value by phthalic anhydride-pyridine method (GB / T12008.3-2009) 25.2mg KOH / g, average molecular weight is 4452.

[0065] The product structure formula is:

[0066]

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Abstract

The invention relates to block oligomeric dihydric alcohol with a controllable structure and a preparation method thereof. The main chain of the block oligomeric dihydric alcohol is a controllable block structure and is obtained by performing propoxylation or ethoxylation / propoxylation on polycarbonate, the terminal group is hydroxyl, the number-average molecular weight is 500-10000, and the molecular weight of carbonate chains and oxidized propylene / ethylene chains is adjustable. The preparation method of the block oligomeric dihydric alcohol comprises the following steps: firstly adding polycarbonate diol and a double-metal cyanide complex catalyst into a reaction kettle, heating to a certain temperature, and performing vacuum dewatering; then adding a part of an epoxide under the condition of 100-180 DEG C to perform an induction reaction, and after the induction reaction is finished, dropwise adding the residual epoxide; and after the reaction is finished, removing the unreacted epoxide to obtain oligomeric dihydric alcohol. The oligomeric dihydric alcohol is mainly applied to synthesis a polyurethane material.

Description

technical field [0001] The invention relates to a block-type oligomeric diol with controllable structure and a preparation method thereof, in particular to a preparation method of a block-type oligomeric diol for preparing polyurethane. Background technique [0002] Polyurethane is a polymer compound obtained by polycondensation reaction of isocyanate and polyol, and the polyol compound mainly includes two categories: polyether polyol and polyester polyol. Polyether polyols or polyester polyols are used as raw materials for synthesizing polyurethanes. Because of their different structures, the polyurethane materials prepared by them have their own advantages and disadvantages. In order to make up for the deficiency in the performance of polyurethane materials prepared by using polyether or polyester polyol alone, people have developed and researched polyether ester products, among which CN101024684A, CN1431240A, US Patent5319006, US Patent20080021154, WO2012022048A1 and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G64/30C08G18/48C08G18/44
Inventor 刘瑞阳陈海波伍燕碧赵晶纪学顺袁银龙刘运海鞠昌迅黄长荣隋宝华李晶丁建生华卫琦
Owner WANHUA CHEM GRP CO LTD
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