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A method for reducing acid value of tdi product by heavy solvent method

A heavy solvent, acid value technology, applied in the purification/separation of isocyanic acid derivatives, organic chemistry, etc., can solve the requirements of reducing the content of acidic components in isocyanate, affecting the stable operation of the reaction yield system, equipment size and energy consumption Advanced problems, to achieve the effect of improving stability, novel design and convenient operation

Active Publication Date: 2017-10-27
QINGDAO UNIV OF SCI & TECH +1
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  • Description
  • Claims
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Problems solved by technology

[0004] The acidic components produced in the process of producing TDI by the heavy solvent method mainly include hydrogen chloride, benzylic chlorotoluene diisocyanate (hereinafter referred to as Cl-TDI), m-ethyl benzoyl chloride (hereinafter referred to as CBC), etc., wherein Cl- The boiling points of TDI and CBC are between the product TDI and the solvent DEIP. In the product refining process, the product and the solvent are separated in the final product tower. On the one hand, if the acidic component is extracted from the tower with the heavy solvent , because the solvent has to be returned to the system for recycling, the presence of acidic components will cause more photochemical side reactions to generate by-products such as residues, which will affect the reaction yield and the stable operation of the system; if the acidic components enter the product If it is extracted from the top of the tower, it is a heavy component compared to TDI. At this time, if the method of rectification or purging is used, a large amount of products will be brought into the gas phase, which requires high equipment size and energy consumption. and cannot reasonably and effectively separate the acidic components
Therefore, the rectification method and gas purging method, which are more suitable for the light solvent method, are not suitable for the removal of acidic components in TDI products produced by the heavy solvent method.
[0005] In addition, in the prior art, there is also a method of reducing the acid value and acidic component content of TDI products by adding additional substances, such as US Pat. Above 180°C, the heating time is preferably above 240min, which can significantly reduce the content of acidic components in isocyanate; although the above method of adding substances can better remove the acidic components in the product, but at the same time introduces a new impurity group After that, it needs to be separated from the product by nitrogen purging, rectification or extraction, which virtually increases the workload

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  • A method for reducing acid value of tdi product by heavy solvent method

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Embodiment 1

[0017] The method for reducing the acid value of the heavy solvent method TDI product involved in the present embodiment is implemented in an acid value reduction device, and the specific process includes the following steps:

[0018] (1) Preheat the photochemical reaction material of toluene diisocyanate (TDI) by the heavy solvent method to 160-190 DEG C through the feed preheater 1 and then send it into the product tower 2, the control pressure is 0.5-20kpaA, and the temperature is 170-240°C; the gas phase in the product tower 2 enters the product tower condenser 3 through the top of the product tower 2, and is condensed at a controlled temperature of 40-100°C, and the non-condensable gas material is extracted from the gas phase at the top of the product tower condenser 3 to the outside The vacuum system of setting, a part of material that condenses is returned in the product tower 2 as reflux through reboiler 4, and the reflux ratio is 1.5~15, and another part of material th...

Embodiment 2

[0025] In this embodiment, the present invention is described in detail by taking specific operation as an example (such as figure 1 Shown): the photochemical reaction stream A containing TDI product, solvent DEIP, acidic components and other impurities with a flow rate of 32680kg / h and an acid value of 67ppm from the previous stage of the process is preheated to 180 through the feed preheater 1 After entering the product tower 2, control the pressure of the product tower 2 to 7kpaA and the temperature of the tower kettle to 215°C; the temperature of the product tower condenser 3 is 60°C for condensation, and the non-condensable gas stream B is extracted in the gas phase to the external vacuum system , TDI product stream C is extracted in liquid phase, the output is 8777kg / h, and the reflux stream D with a reflux ratio of 2.5 is returned to the product tower 2 as reflux through the reboiler 4; the acid value extracted from the product tower 2 The solvent DEIP stream E of 84ppm...

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Abstract

The invention belongs to the technical filed of chemical production and relates to a method for reducing the acid value of a toluene diisocaynate (TDI) product prepared through a heavy solvent method. Photochemical reaction materials of the TDI prepared through the heavy solvent method are sent to a product tower after undergoing preheating of a feeding preheater, a gas phase inside the product tower enters a product tower condenser from the top of the product tower to perform condensation, the gas phase of a noncondensable gas material is extracted to be vacuum, part of the condensed materials serve as backflow, and the other part of the condensed materials serve as TDP product liquid phase to be extracted. DEIP extracted from the product tower is sent to a blowing tower after undergoing pressure boosting of a kettle liquid pump, is sprayed to the blowing tower after the distribution of a distribution device, flows under the effect of gravity and is fully in contact with inert gas blowing into the blowing tower. Acid components in the DEIP gather at the top of the blowing tower along with the inert gas and enter a blowing tower condenser in a gas phase mode to be condensed, the gas phase of the noncondensable gas material is extracted to be vacuum, the condensed acid components pass through the bottom of the blowing tower condenser to be extracted in a liquid phased mode, and recycling solvent of a small acid value is obtained from the bottom of the blowing tower. The method is novel in design, scientific in principle and simple in technology.

Description

Technical field: [0001] The invention belongs to the technical field of chemical production, and relates to a method for reducing the acid value of TDI products produced by a heavy solvent method, which can reduce the generation of by-products when the circulating solvent returns to the previous process to participate in the photochemical reaction, thereby improving the efficiency of the photochemical reaction and the stability of the system sex. Background technique: [0002] Toluene diisocyanate (hereinafter referred to as TDI) is an important isocyanate product. Common production and preparation methods in the industry include phosgenation, nitro compound carbonylation and dimethyl carbonate. Among them, phosgenation is generally The following two processes are used: one is to use diethyl isophthalate (hereinafter referred to as DEIP) as a solvent, and carry out photochemical reaction under high pressure conditions, which is called "heavy solvent method"; Chlorobenzene (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C263/20C07C265/14
CPCC07C263/20C07C265/14
Inventor 毕荣山张波葛纪军韩传贵曾民成谭心舜郑世清
Owner QINGDAO UNIV OF SCI & TECH
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