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A kind of heat-sensitive catalyst for solvent-free polyurethane synthesis and preparation method thereof

A heat-sensitive catalyst and solvent-free polyurethane technology, applied in organic chemistry and other fields, can solve problems such as environmental and human hazards, affecting material properties, etc.

Active Publication Date: 2018-07-20
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All of the above methods can play a good role in delaying the catalyst, but they will release or leave inhibitors in the polyurethane material or the environment. Inhibitors in polyurethane materials can seriously affect the performance of the material

Method used

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  • A kind of heat-sensitive catalyst for solvent-free polyurethane synthesis and preparation method thereof
  • A kind of heat-sensitive catalyst for solvent-free polyurethane synthesis and preparation method thereof
  • A kind of heat-sensitive catalyst for solvent-free polyurethane synthesis and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Preparation of Example 1 Compound 1 Sample A

[0085]Add 1.5224g (10mmol) of 1,8-diazabicycloundec-7-ene into a dry single-necked bottle, place it in a low-temperature (-15°C) reaction device, and then add 10ml of anhydrous diethyl ether with a magnetic stirrer Mix and dissolve 1,8-diazabicycloundec-7-ene completely, add 2.6629g (20mmol) of benzyl isocyanate into a 25ml constant pressure dropping funnel, and use constant pressure dropping Slowly add benzyl isocyanate into the above solution through a funnel under magnetic stirring. After the addition is completed, stir rapidly for 5 minutes. After the reaction is completed, a large amount of solids will precipitate out. The recrystallized solid was filtered, then washed 2-3 times with frozen ether, and then dried under vacuum at 90°C for 4-5 hours. The obtained product was Compound 1, which was recorded as sample A, and the obtained product was placed in a dry sealed system Store in a dry environment until use.

[008...

Embodiment 2

[0088] Preparation of Example 2 Compound 1 Sample B

[0089] Add 1.2418g (10mmol) of 1,5-diazabicyclo[4,3,0]nonene-5 to a dry one-necked bottle, place it in a low-temperature (-10°C) reaction device, and then add 10ml of Mix and dissolve 1,5-diazabicyclo[4,3,0]nonene-5 with water and ether magnetically, add 2.5298g (19mmol) of benzyl isocyanate to a 25ml constant pressure dropping funnel Among them, use a constant pressure dropping funnel to slowly add benzyl isocyanate into the above solution under magnetic stirring, and stir rapidly for 10 minutes after the addition is completed. After the reaction is completed, a large amount of solids will precipitate out. Recrystallize in a low-temperature device, filter the recrystallized solid, wash with frozen ether 2 to 3 times, and then dry at 90°C under vacuum for 4 to 5 hours. The obtained product is compound 1, which is designated as sample B. The obtained product is packed into a dry sealed system and stored in a dry environment...

Embodiment 3

[0090] Preparation of Example 3 Compound 1 Sample C

[0091] Add 1.5322g (10mmol) of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene into a dry one-necked bottle, and place it in a low temperature (0°C) reaction device , then add 10ml of anhydrous ether and magnetically stir to make 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene mixed and dissolved completely, and 2.6629g (19mmol) of isocyanide Add benzyl isocyanate into a 25ml constant-pressure dropping funnel, slowly add benzyl isocyanate into the above solution under magnetic stirring using the constant-pressure dropping funnel, and stir rapidly for 15 minutes after the addition is completed. After the reaction is completed, there will be a large amount of The solid precipitated, put the reaction bottle into a low-temperature device at -30°C for recrystallization, filtered the recrystallized solid, washed it with frozen ether for 2 to 3 times, and then dried it under vacuum at 90°C for 4 to 5 hours to obtain the product That is...

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Abstract

The invention discloses a temperature-sensitive catalyst used for solvent-free polyurethane synthesis, and a preparation method thereof. The temperature-sensitive catalyst used for solvent-free polyurethane synthesis is characterized in that the temperature-sensitive catalyst includes a compound 1, a compound 2 and a compound 3; the compound 1 is selected from a compound with the chemical structural formula of formula I-1, a compound with the chemical structural formula of formula I-2 and a compound with the chemical structural formula of formula I-3; the compound 2 is selected from at least one of compounds with the chemical structural formula of formula II; and the compound 3 is selected from at least one of compounds with the chemical structural formula of formula III. The temperature-sensitive catalyst is used for preparing solvent-free polyurethane materials, and has the characteristics of low temperature retardance, low volatility, and satisfactory balancing of the foaming rate and the gelling rate.

Description

technical field [0001] The application relates to a heat-sensitive catalyst for the synthesis of solvent-free polyurethane, which belongs to the field of polyurethane material synthesis. Background technique [0002] Polyurethane is a general term for macromolecular compounds containing repeated carbamate groups in the main chain, and is widely used in various industries of life and industrial production because of its special physical and chemical properties. Polyurethane is mainly formed by addition polymerization of organic diisocyanate or polyisocyanate, dihydroxy or polyhydroxy compound and other additives under certain reaction conditions (Polymer, 2015, 56:37-45; Polymer, 2015, 56:93-101 ). Foremost among these additives are catalysts. On the one hand, catalysts can greatly increase the reaction rate, which is a necessary condition for improving production efficiency and obtaining high molecular weight polyurethane; on the other hand, the use of different catalysts ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/20C08G18/66C08G18/44C08G18/48C07D487/20
CPCC07D487/20C08G18/2072C08G18/4018C08G18/44C08G18/4854C08G18/664C08G18/6674
Inventor 李文木苏玉苗
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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