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Polyether polyol for flame-retardant polyurethane rigid foam and preparation method thereof

A technology of polyether polyol and polyurethane rigid foam is applied in the field of polyether polyol for flame retardant polyurethane rigid foam and its preparation, which can solve the problems of influence of polyether polyol performance, low flame retardant efficiency and high cost, and achieves Overcome inherent defects, excellent flame retardant effect, and solve the effect of poor durability

Active Publication Date: 2019-05-10
CHENGDU TEXTILE COLLEGE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing polyurethane rigid foam flame retardant method, one is additive flame retardant, the defect of this method is that with the increase of the service life of the rigid foam, the flame retardant will be precipitated from the rigid foam, which will affect the performance of the rigid foam; Another method is the modification of raw materials. One is the flame-retardant modification of isocyanate. At present, only a few countries such as Japan produce flame-retardant isocyanate in small batches, and the flame-retardant effect is not obvious; the other is for polyether The flame-retardant modification of polyols, however, the modification method of polyether polyols in the prior art often has the following disadvantages: the introduction of halogen-containing compounds, and the combustion of halogen-containing compounds is easy to produce carcinogenic and corrosive gases, which is harmful to The harm to the human body and the environment is great; the introduction of phosphate ester content is large, which affects the performance of polyether polyol itself, and the cost is high; the flame retardant efficiency of introducing N element into polyether polyol is not high

Method used

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  • Polyether polyol for flame-retardant polyurethane rigid foam and preparation method thereof
  • Polyether polyol for flame-retardant polyurethane rigid foam and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This embodiment provides a preparation method of polyether polyol for flammable polyurethane rigid foam:

[0028] (1) Crude flame-retardant polyether polyol: Add 133g polyphosphoric acid and 270g (1:2) pentaerythritol into a 3L autoclave under the conditions of 60°C and 1MPa, and react under reflux for 3h to obtain the first mixture; Then add 75g (3.6) glycerol and 10g potassium hydroxide to the first mixture, stir and raise the temperature to form a second mixture, blow in nitrogen for 3 times, vacuum to remove water; then raise the temperature to 90°C and control the reaction pressure to 0.1 MPa, 540g (2:1) of ethylene oxide is added to the second mixture by continuous feeding, then the temperature is raised to 110°C, the temperature is kept for 2h, and the reaction pressure is controlled to 0.05-0.1MPa for reaction to obtain crude flame retardant Polyether polyol;

[0029] (2) Refined flame-retardant polyether polyol: After adding 1.5% of its own mass of phosphoric acid ...

Embodiment 2

[0031] This embodiment provides a preparation method of polyether polyol for flammable polyurethane rigid foam:

[0032] (1) Crude flame-retardant polyether polyol: Add 135g of polyphosphoric acid and 337g of pentaerythritol to a 3L autoclave at 70°C and 1MPa, and react under reflux for 3h to obtain the first mixture; Add 85g of sorbitol, 10g of potassium hydroxide, stir and raise the temperature to form a second mixture, blow in nitrogen for 3 times, vacuum to remove water; then raise the temperature to 100°C, control the reaction pressure to 0.1MPa, and use continuous Adding 1011g of propylene oxide in the way of feeding, then heating to 110°C, holding for 2h, controlling the reaction pressure to 0.05-0.1MPa for reaction, and obtaining crude flame-retardant polyether polyol;

[0033] (2) Refined flame-retardant polyether polyol: After adding 1.5% of its own mass of phosphoric acid and 0.8% of adsorbent to the crude flame-retardant polyether polyol, it is filtered and dried.

experiment example 1

[0047] Take equal amounts of the polyether polyols provided in Examples 1-2 and Comparative Examples 1-3 and set them as experimental groups 1-5, and perform performance characterization and application characterization of experimental groups 1-5 as follows:

[0048] 1.1 Performance characterization

[0049] (1) Determination of hydroxyl value: Weigh 2.0 g (accurate to 0.0001 g) of a sample into an iodine flask, add 15 mL of acetylation reagent to it, and mix well to dissolve the sample completely. React in a water bath at 60°C for 30 minutes, take it out, and cool to room temperature, then add 20 mL of pyridine solution, 2 drops of phenolphthalein indicator, and titrate with NaOH standard solution until the solution turns pink. The end of the titration is that the color does not fade within 15 seconds. At the same time, a blank test is performed, and the hydroxyl value calculation formula is as follows:

[0050] Hydroxyl value / mgKOH.g -1 =(V 1 -V 2 )c×56.1 / m

[0051] Where: V 1 -The...

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Abstract

The invention relates to the technical field of flame retardant modification, and provides polyether polyol for flame-retardant rigid polyurethane foam and a preparation method thereof. The preparation method comprises the following steps: (1) coarsely preparing flame-retardant polyether polyol, namely mixing polyphosphoric acid and pentaerythritol to perform a reflux reaction to obtain a first mixture; then, adding polyol and potassium hydroxide into the first mixture, reacting to form a second mixture, and vacuumizing and dehydrating the second mixture; heating, controlling the reaction pressure, adding an epoxy compound into the second mixture, heating, and controlling the reaction pressure to react to obtain the coarsely prepared flame-retardant polyether polyol; and (2) refining the flame-retardant polyether polyol, namely adding phosphoric acid and adsorbent into the coarsely prepared flame-retardant polyether polyol, filtering and drying. The preparation method is simple in synthesis process and low in cost, and can be used for preparing the polyether polyol with excellent flame retardant performance.

Description

Technical field [0001] The invention belongs to the technical field of flame retardant modification, and specifically relates to a polyether polyol for flame-retardant polyurethane rigid foam and a preparation method thereof. Background technique [0002] Polyurethane is the abbreviation of polyurethane, which is a general term for a type of polymer with repeating carbamate groups on the main chain prepared by the reaction of polyols and polyisocyanates. Rigid polyurethane foam is one of the largest products in the polyurethane industry. Because of its light weight, high specific strength and excellent thermal insulation performance, it is widely used in the field of thermal insulation materials. However, non-flame retardant polyurethane rigid foams have a limiting oxygen index of less than 20% and are extremely combustible. The production of toxic gases CO and HCN after combustion are often the direct causes of people's suffocation and poisoning deaths in fires. [0003] Therefor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/327C08G65/28C08G18/50C08G101/00
CPCC08G18/5075C08G65/2609C08G65/327C08G2110/0025
Inventor 陈荣义黄剑袁明强何杰
Owner CHENGDU TEXTILE COLLEGE