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Preparation method and application of isocyanate

A technology of isocyanate and nylon acid, applied in the preparation of carboxylic acid nitrogen-containing derivatives, non-polymer adhesive additives, adhesive additives, etc., can solve the problems of large waste water, low recovery rate, environmental pollution, etc., and achieve reduction The effect of interfacial tension, high production efficiency, and easy post-processing operation

Inactive Publication Date: 2015-07-15
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recrystallization method is used for purification and recovery, the recovery rate is lower than 60%, and the amount of waste water is large, which not only pollutes the environment, but also causes serious waste of resources; adopts distillation method for separation, and all decompose when it is close to the boiling point

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of isocyanate

[0029] (1) 60 parts by mass of urea, while stirring, add 35 parts by mass of nylon acid. When the temperature reaches 140°C, the urea melts for 10 minutes. A large amount of gas is released. The temperature is raised to 170°C and kept for 4 hours. Cool to 110℃, under vigorous stirring, add 350 parts by mass of 5% sodium carbonate solution dropwise, cool in an ice bath, filter and dry to obtain C 4-6 Aliphatic amide, product yield 87%;

[0030] (2) Take 60 parts by mass of C 4-6 Aliphatic amide, add 250 parts by mass of chlorobenzene, cool to 0-2°C in an ice bath, add 320 parts by mass of oxalyl chloride at a time under stirring, and stir for 10 min; remove the ice bath, stir at room temperature for 1 h, and heat to reflux for 5 h. Distill under reduced pressure to obtain isocyanate; said isocyanate is C 4-6 Aliphatic amide isocyanate, the yield is 65%, and the mass fraction of free isocyanate groups is 32%.

[0031] Said nylon acid...

Embodiment 2

[0033] A kind of preparation method of isocyanate

[0034] (1) 60 parts by mass of urea, while stirring, add 45 parts by mass of nylon acid. When the temperature reaches 140°C, the urea melts for 10 min. A large amount of gas is released. Raise the temperature to 180°C and keep the mixture for 4 hours. Cool to 120℃, under vigorous stirring, add dropwise 400 mass parts of sodium carbonate solution with mass fraction of 5%, cool in an ice bath, filter, and dry to obtain C 4-6 Aliphatic amide, product yield is 91%;

[0035] (2) Take 60 parts by mass of C 4-6 Aliphatic amide, add 250 parts by mass of dichloroethane, cool to 0-2℃ in an ice bath, add 320 parts by mass of oxalyl chloride at a time while stirring, and stir for 10 min; remove the ice bath, stir at room temperature for 1 h, and heat to reflux 5h, distillation under reduced pressure to obtain isocyanate; said isocyanate is C 4-6 Aliphatic amide isocyanate, the yield is 70%, and the mass fraction of free isocyanate groups is 3...

Embodiment 3

[0038] A kind of preparation method of isocyanate

[0039] (1) 60 parts by mass of urea, while stirring, add 35-45 parts by mass of nylon acid. When the temperature reaches 140°C, the urea melts for 10 minutes. A large amount of gas is released. The temperature is raised to 175°C and kept for 4 hours. The mixture was cooled to 115°C, under vigorous stirring, 375 parts by mass of sodium carbonate solution with a mass fraction of 5% was added dropwise, cooled in an ice bath, filtered, and dried to obtain C 4-6 Aliphatic amide, product yield is 89%;

[0040] (2) 60 parts by mass of C 4-6 Aliphatic amide, add 230 parts by mass of xylene, cool to 0-2°C in an ice bath, add 300 parts by mass of oxalyl chloride at a time while stirring, and stir for 10 min; remove the ice bath, stir at room temperature for 1 h, and heat to reflux for 5 h. Distill under reduced pressure to obtain isocyanate; said isocyanate is C 4-6 Aliphatic amide isocyanate, the yield is 67%; the mass fraction of free iso...

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PUM

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Abstract

The invention relates to a preparation method and application of isocyanate, particularly relates to a preparation method of C4-C6 aliphatic isocyanate prepared from nylon acid as a raw material, and an application of the C4-C6 aliphatic isocyanate, and belongs to the technical fields of organic synthesis, adhesive chemistry and composite materials. The C4-C6 aliphatic isocyanate is prepared from urea and nylon acid as raw materials in manners of firstly preparing C4-6 aliphatic amide and reacting the C4-6 aliphatic amide with oxalyl chloride. The isocyanate is applied to preparation of polyurethane foaming plastic, rubber, elastic fibers, coatings, and bonding wood based composite materials.

Description

Technical field [0001] The invention relates to a preparation method and application of isocyanate, in particular to a preparation method and application of isocyanate prepared with nylon acid as a raw material, and belongs to the technical fields of organic synthesis, adhesive chemistry and composite materials. Background technique [0002] Substances containing highly reactive free unsaturated isocyanate groups (-NCO) in the molecule are called isocyanates. According to the number of free -NCO in the molecule, isocyanates can be divided into monoisocyanate R-NCO, diisocyanate OCN-R-NCO and two Above-NCO polyisocyanate. Isocyanates are very easy to react with some organic or inorganic substances with active functional groups, for example, react with hydroxyl compounds to form aminomethyl esters; react with amine compounds to form substituted ureas, which further react to form biurets; react with water Amine and carbon dioxide are formed. The amine further reacts with isocyanate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C265/16C07C263/12C08G18/78C09J11/06
Inventor 王志玲郑鲁沂张书香黄晓丽崔恩峰李海芳田亮
Owner UNIV OF JINAN
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