Method for continuously preparing 1,5-naphthalene diisocyanate

A technology of carbonate and diaminonaphthalene, which is applied in the field of continuous preparation of 1,5-naphthalene diisocyanate, can solve the problems of small production capacity of a single reactor, unstable product quality, and low utilization rate of equipment, and achieve improved production operations The environment, production capacity is easy to enlarge, and the effect of short reaction time

Inactive Publication Date: 2013-07-24
XIANGTAN UNIV
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Problems solved by technology

[0009] The present invention is aimed at the existing process for preparing 1,5-naphthalene diisocyanate, most of which adopt intermittent production mode, which has long reaction time, low equipment utilization rate, low yield, unstable product quality, and small production capacity of a single reactor etc., the purpose is to provide a method for preparing 1,5-naphthalene diisocyanate with high yield, high purity, low cost, short reaction time, high equipment utilization, no pollution, and continuous industrial production

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  • Method for continuously preparing 1,5-naphthalene diisocyanate

Examples

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Effect test

Embodiment 1

[0022] The chlorobenzene solution of 1,5-diaminonaphthalene with a concentration of 3g / 100mL and the chlorobenzene solution of 20g / 100mL bis(trichloromethyl)carbonate, according to the concentration of bis(trichloromethyl)carbonate and 1,5 - The molar ratio of diaminonaphthalene is 1.5:1. After mixing in a Venturi mixer, it enters a tubular reactor for 0.1 minutes. After the reaction temperature rises to 70°C, it enters a series of 6-stage stirred tank reactors. Combined reactor reaction, the temperature of the first-stage stirred tank reactor is controlled at 70 °C, the temperature of the next-stage stirred tank reactor is increased by 10 °C, and the temperature of the last-stage stirred tank reactor is controlled at 130 °C ℃ reaction, the total residence time of the reactor is controlled to be 6 hours, after the material is completely reacted, it is filtered, and the filtrate is concentrated and crystallized to obtain 99.1% of 1,5-naphthalene diisocyanate; the yield of 1,5-na...

Embodiment 2

[0024] Dimethyl carbonate solution of 1,5-diaminonaphthalene with a concentration of 10g / 100mL and dimethyl carbonate solution of bis(trichloromethyl)carbonate at a concentration of 5g / 100mL, according to bis(trichloromethyl)carbonate The molar ratio with 1,5-diaminonaphthalene is 2:1. After mixing at the inlet of the pipeline pump, it enters a tubular reactor for reaction for 5 minutes. After the reaction temperature rises to 90°C, it enters a stirred tank type reactor consisting of 3 stages in series. For reactor reaction, the temperature of the first-stage stirred tank reactor is controlled at 90°C, the temperature of the second-stage stirred tank reactor is controlled at 105°C, and the temperature of the third-stage stirred tank reactor is controlled at 130°C. The total residence time of the reactor is controlled to be 8 hours. After the material is completely reacted, it is filtered, and the filtrate is concentrated and crystallized to obtain 98.1% of 1,5-naphthalene diiso...

Embodiment 3

[0026] The chlorobenzene solution of 1,5-diaminonaphthalene with a concentration of 6g / 100mL and the chlorobenzene solution of 20g / 100mL bis(trichloromethyl)carbonate, according to the concentration of bis(trichloromethyl)carbonate and 1,5 - The molar ratio of diaminonaphthalene is 1.5:1. After mixing in a static mixer, it enters a tubular reactor for 1.5 minutes. After the reaction temperature rises to 70°C, it enters a combination of 6-stage stirred tank reactors in series. Reactor reaction, the temperature of the first stirred tank reactor is controlled at 70°C, the temperature of the next stirred tank reactor is increased by 10°C, and the temperature of the last stirred tank reactor is controlled at 130°C For the reaction, the total residence time of the reactor is controlled to be 5 hours. After the material is completely reacted, it is filtered, and the filtrate is concentrated and crystallized to obtain 99.3% of 1,5-naphthalene diisocyanate, and the yield of 1,5-naphthal...

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Abstract

The invention discloses a method for continuously preparing 1,5-naphthalene diisocyanate, and the method comprises the following steps of: firstly mixing a 1,5-naphthalene diisocyanate solution and a di(trichloromethyl) carbonate solution into a reaction raw material, and then carrying out continuous charging; enabling the reaction raw material to firstly flow through a tubular reactor at the temperature of 25-100 DEG C and then flow through 3-8 stage series-connected combined slot type reactors, and enabling an obtained mixture to flow out of the last-stage reactor; and filtering, and then concentrating and crystallizing filter liquor to obtain the 1,5-naphthalene diisocyanate. The method disclosed by the invention has the advantages of high reaction yield, high product purity, short reaction time, high equipment utilization ratio, low production cost, no pollution, continuous production and industrialized application.

Description

technical field [0001] The invention relates to a method for continuously preparing 1,5-naphthalene diisocyanate, which belongs to the field of organic synthesis. Background technique [0002] 1,5-Naphthalene diisocyanate (NDI) is an important intermediate for the synthesis of polyurethane materials with excellent properties. The polyurethane material based on 1,5-naphthalene diisocyanate has the characteristics of high hardness, good resilience, excellent dynamic performance and good wear resistance. It is used in large machinery, new rail transit equipment, shock absorption and noise prevention, new energy wind power Composite materials for equipment blades, new thin film materials for solar cell new energy, tires for automobiles and forklifts, springs and shock absorbers play a very critical role. [0003] At present, the synthesis routes of NDI mainly include phosgene method (GB761594; GB1142628; GB1173890) and non-phosgene method. The phosgene method uses 1,5-diaminon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/14C07C263/10
Inventor 艾秋红罗和安袁峰王良芥游奎一刘平乐黄荣辉
Owner XIANGTAN UNIV
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