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Method for purifying triisocyanate

A technology for purifying triisocyanates and triisocyanates, applied in chemical instruments and methods, purification/separation of isocyanate derivatives, organic chemistry, etc., can solve the problems of harsh reaction conditions, high cost, long-term high-temperature synthesis, etc. Good stability and the effect of enhancing adsorption capacity

Active Publication Date: 2022-02-18
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Therefore, the current synthesis methods of functionalized porous polymer materials mainly have the following defects: (1) the introduction of active groups into porous polymers cannot be reasonably realized; (2) the synthesis process mainly uses noble metals (such as Pd, Au) as catalysis, and requires long-term high-temperature synthesis
There are problems such as high cost, low efficiency and harsh reaction conditions in the synthesis process
[0005] Considering the limited introduction of active groups, low synthesis efficiency, and high cost during the synthesis of functionalized porous polymers, the technical problem that needs to be urgently solved by those skilled in the art is: adopting a reasonable active group to introduce porous polymers method for the synthesis of porous polymers using inexpensive starting materials, high efficiency, and mild reaction conditions
[0006] Considering that the commonly used method for purifying isocyanate cannot meet our requirements for purifying triisocyanate, the technical problem that needs to be urgently solved by those skilled in the art is: to adopt a method that has good thermal stability, effectively reduces production energy consumption, and reduces environmental pollution. The method to purify triisocyanate, especially to purify high boiling point, dark color triisocyanate containing impurities, to make it transparent

Method used

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  • Method for purifying triisocyanate
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  • Method for purifying triisocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0114] Example 1 Preparation of Exo-configuration polynorbornene imide porous material Ⅰ-a

[0115] Step 1: Preparation of Exo-configuration norbornene imide monomer Ⅱ-a

[0116]

[0117] Weigh 1,3,5-triaminobenzene hydrochloride (1.23g, 10.0mmol, 1.0equiv.) and exo-norbornene anhydride (5.4g, 33.0mmol, 1.1equiv.) in a 250mL single-necked flask, Toluene (100 mL) and triethylamine (3 mL) were added respectively, and the temperature was raised to 135°C for heating; the reaction solution changed from cloudy to clear at the beginning, and precipitates gradually precipitated as the reaction progressed. After reacting for 5 hours, cool to room temperature, and carry out suction filtration under reduced pressure; add water and ethanol to wash the filter cake for 2-3 times, heat and dry to obtain off-white solid (5.41g, 96% yield).

[0118] 1 H NMR (400MHz, CDCl 3 )δ (ppm): 7.48 (s, 3H), 6.35 (s, 6H), 3.40 (s, 6H), 2.85 (s, 6H), 1.62 (d, J = 10.0Hz, 3H), 1.47 (d, J = 10.0Hz, 3H...

Embodiment 2

[0123] Example 2 Preparation of Exo-configuration polynorbornene imide porous material Ⅰ-b

[0124] Step 1: Preparation of Exo-configured norbornene imide monomer II-b

[0125]

[0126] Weigh three (4-aminophenyl) methane (2.9g, 10.0mmol, 1.0equiv.) and exo-norbornene anhydride (5.4g, 33mmol, 1.1equiv.) in a 250mL single-necked flask, add toluene ( 100mL) and triethylamine (3mL), heated to 130°C; the reaction solution changed from cloudy to clear at the beginning, and precipitates gradually precipitated as the reaction progressed. After reacting for 6 hours, it was cooled to room temperature and subjected to suction filtration under reduced pressure; the filter cake was washed with water and ethanol for 2-3 times, then heated and dried to obtain a light white solid (7.02g, 91% yield).

[0127] 1 H NMR (400MHz, CDCl 3 )δ (ppm): 7.22 (s, 12H), 6.35 (t, J = 1.9Hz, 6H), 5.62 (s, 1H), 3.43–3.39 (m, 6H), 2.86 (d, J = 1.2Hz, 6H), 1.62(d, J=9.9Hz, 3H), 1.47(d, J=9.9Hz, 3H); 13...

Embodiment 3

[0132] Example 3 Preparation of Exo-configuration polynorbornene imide porous material I-c

[0133] Step 1: Preparation of Exo-configured norbornene imide monomer II-c

[0134]

[0135] Weigh three (4-aminophenyl) triazine (3.54g, 10.0mmol, 1.0equiv.) and exo-norbornene anhydride (5.4g, 33mmol, 1.1equiv.) in a 250mL single-necked flask, add toluene respectively (100mL) and triethylamine (3mL), heated to 130°C; the reaction solution changed from cloudy to clear at the beginning, and precipitates gradually precipitated as the reaction progressed. After reacting for 6 hours, cool to room temperature, and carry out suction filtration under reduced pressure; add water and ethanol to wash the filter cake for 2-3 times, heat and dry to obtain a light white solid (7.4g, 93% yield).

[0136] 1 H NMR (400MHz, CDCl 3 )δ (ppm): 8.84 (d, J = 8.2Hz, 6H), 7.54 (d, J = 8.3Hz, 6H), 6.40 (s, 6H), 3.47 (s, 6H), 2.93 (s, 6H) ,1.68(d,J=10.0Hz,3H),1.56(d,J=10.0Hz,3H); 13 CNMR (100MHz, CDCl ...

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Abstract

The invention discloses a method for purifying triisocyanate, which is characterized in that a polynorbornene imide porous material is used as a solid adsorbent to purify the triisocyanate, so that the triisocyanate is transparent. Specifically, the polynorbornene imide porous material provided by the invention combines an imide functional group with a polynorbornene skeleton structure, and has the characteristics of a micropore-mesopore hierarchical pore structure mainly comprising micropores, so that the polynorbornene imide porous material has rich functional groups, high specific surface area, larger total pore volume and smaller average pore size, and plays an important role in the fields related to environment and energy such as organic pollutant adsorption, heterogeneous catalysis, gas storage and the like. In addition, the porous material provided by the invention has excellent performance of good thermal stability, so that the porous material has potential application prospects.

Description

technical field [0001] The present invention relates to the field of novel organic porous polymer materials and polyisocyanates, and mainly relates to a method for purifying triisocyanates. Background technique [0002] Polyisocyanates are a class of chemicals that contain active groups and are closely related to human life. However, the purification of polyisocyanate products is still a great challenge (Angew.Chem.Int.Ed., 2013, 52, 9422-9441; Chem. Rev., 2013, 113, 80-118; RSCAdvances, 2016, 6, 114453-114482). At present, vacuum distillation is mainly used to purify isocyanate, which not only consumes high energy and has low efficiency, but also is not suitable for the purification of high-boiling triisocyanate (such as lechner gum, etc.). Therefore, it is very important to find a method suitable for purifying polyisocyanates at room temperature. Among them, the development of porous adsorbent materials that selectively adsorb impurities in polyisocyanate products is an ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/20C07C265/14B01J20/26B01J20/30C08G61/12
CPCC07C263/20C08G61/124B01J20/262C08G2261/3241C08G2261/418C07C265/14
Inventor 黄木华彭山青张志豪杨天宇刘艳
Owner BEIJING INSTITUTE OF TECHNOLOGYGY