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Preparation method and application of isocyanate

An isocyanate, nylon acid technology, applied in the preparation of carboxylic acid nitrogen-containing derivatives, non-polymer adhesive additives, adhesive additives and other directions, can solve the problems of large amount of waste water, waste of resources, low recovery rate, etc. Effects of interfacial tension, increased production efficiency, and high production efficiency

Inactive Publication Date: 2014-04-16
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, under stirring, add 35 parts by mass of nylon acid. When the temperature reaches 140°C, the urea melts and lasts for 10 minutes. A large amount of gas is released. Raise the temperature to 170°C and keep it warm for 4 hours. Cooled to 110 ° C, under vigorous stirring, dropwise added 350 parts by mass of sodium carbonate solution with a mass fraction of 5%, cooled in an ice bath, filtered, and dried to obtain C 4-6 Aliphatic amide, product yield 87%;

[0030] (2) Take 60 mass parts of C 4-6 For aliphatic amides, add 250 parts by mass of chlorobenzene, cool in an ice bath to 0-2°C, add 320 parts by mass of oxalyl chloride once under stirring, and stir for 10 minutes; remove the ice bath, stir at room temperature for 1 hour, and heat to reflux for 5 hours. Underpressure distillation, makes isocyanate; Described isocyanate is C 4-6 Aliphatic amide isocyanate, the yield is 65%, and the mass ...

Embodiment 2

[0033] A kind of preparation method of isocyanate

[0034] (1) 60 parts by mass of urea, under stirring, add 45 parts by mass of nylon acid. When the temperature reaches 140°C, the urea melts and lasts for 10 minutes. A large amount of gas is released. Raise the temperature to 180°C and keep it warm for 4 hours. Cooled to 120 ° C, under vigorous stirring, dropwise added 400 parts by mass of sodium carbonate solution with a mass fraction of 5%, cooled in an ice bath, filtered, and dried to obtain C 4-6 Aliphatic amide, product yield 91%;

[0035] (2) Take 60 mass parts of C 4-6 For aliphatic amides, add 250 parts by mass of dichloroethane, cool in an ice bath to 0-2°C, add 320 parts by mass of oxalyl chloride once while stirring, and stir for 10 minutes; remove the ice bath, stir at room temperature for 1 h, and heat to reflux 5h, underpressure distillation, makes isocyanate; Described isocyanate is C 4-6 Aliphatic amide isocyanate, the yield is 70%, and the mass fraction of...

Embodiment 3

[0038] A kind of preparation method of isocyanate

[0039] (1) 60 parts by mass of urea, under stirring, add 35-45 parts by mass of nylon acid, when the temperature reaches 140°C, the urea melts, lasts for 10 minutes, a large amount of gas is released, raise the temperature to 175°C, keep it for 4 hours, The mixture was cooled to 115°C, and 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 89%;

[0040] (2) 60 parts by mass of C 4-6 For aliphatic amide, add 230 parts by mass of xylene, cool in an ice bath to 0-2°C, add 300 parts by mass of oxalyl chloride once under stirring, and stir for 10 minutes; remove the ice bath, stir at room temperature for 1 hour, and heat to reflux for 5 hours. Underpressure distillation, makes isocyanate; Described isocyanate is C4-6 The yield of aliphatic amide isocyanate is 67%; the mass ...

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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 from nylon acid, and belongs to the technical fields of organic synthesis, adhesive chemistry and composite materials. Background technique [0002] The substance containing highly active free unsaturated isocyanate group (-NCO) in the molecule is called isocyanate. According to the number of free -NCO in the molecule, isocyanate can be divided into monoisocyanate R-NCO, diisocyanate OCN-R-NCO and two The above-NCO polyisocyanates. Isocyanate is very easy to react with some organic or inorganic substances with active functional groups, for example, react with hydroxyl compounds to form carbamate; react with amine compounds to form substituted urea, and the substituted urea further reacts to finally form biuret; react with water Amine and carbon dioxide are generated, and the amine further reacts with...

Claims

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Application Information

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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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