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Recovery method of organic amine
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A recovery method, a technology of a manufacturing method, applied in the field of active ingredients, capable of solving problems such as clogging
Active Publication Date: 2022-06-28
ASAHI KASEI KK
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[0006] In addition, when the composition containing the above-mentioned by-products is a highly viscous liquid or solid at around room temperature, clogging, etc. may occur in the continuous production of isocyanate compounds.
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Embodiment 1
[0436] Step (1-A): A step of obtaining a liquid phase component containing a high boiling point compound by-produced in the production of compound (I)
[0437] (Manufacture of urethane)
[0438] use Figure 12 device shown.
[0439] A mixture of 9.8 kg of 2,4-toluenediamine, 10.3 kg of urea, and 261.9 kg of 4-(1,1,3,3-tetramethylbutyl)phenol was supplied to the continuous multistage distillation at 90 kg / Hr through line A1 Tower A101.
[0440] The continuous multistage distillation column A101 is an apparatus for carrying out the urethane-forming step, and the column bottom temperature was set to 250° C. and the column top pressure was set to 5 kPa by heating with the reboiler A111.
[0441] The reaction liquid was discharged at 90.7 kg / Hr from the bottom of the continuous multistage distillation column A101.
[0442] The gas-phase components were discharged from the top of the continuous multistage distillation column A101, and introduced into the condenser A103 through t...
Embodiment 2
[0476] Process (2-A)
[0477] (Manufacture of urethane)
[0478] use Figure 13 The apparatus shown carries out the urethanization step. A mixture of 11.3 kg of 1-amino-3-aminomethyl-3,5,5-trimethylcyclohexane, 15.1 kg of urea, and 220.3 kg of 1-butanol was fed to a continuous multistage at 20 kg / Hr from line A21 Distillation column A201. 1-Butanol is suitably fed from line A25.
[0479] The gas phase components produced in the continuous multistage distillation column A201 are introduced into the condenser A203 through the line A23. The gas phase component introduced into the condenser A203 was cooled to 0° C. to obtain a mixed liquid of 1-butanol and urea. A part of this mixed liquid was supplied to the continuous multistage distillation column A201 at 3.5 kg / Hr from the line A24, and the rest was recovered to the storage tank A204.
[0480] The continuous multistage distillation column A201 is an apparatus for carrying out the urethane-forming step, and the column bot...
Embodiment 3
[0512] Step (3-A): A step of obtaining a liquid phase component containing a high boiling point compound by-produced in the production of compound (I)
[0513] (Manufacture of urethane)
[0514] use Figure 16 device shown.
[0515] 50 kg of phenol was supplied to stirring tank A501 through line 50, and then 38 kg of diphenyl carbonate was supplied to prepare a uniform solution. 15 kg of 4,4'-dicyclohexylmethanediamine was gradually added to the stirring tank A501 while maintaining the temperature at 40°C. After the addition was terminated, stirring was continued for 5 hours, after which the reaction solution was transferred to the storage tank 502 through the line A51.
[0516] (Thermal decomposition of urethane)
[0517] The same method as the "thermal decomposition of urethane" of Example 2 was carried out to obtain dicyclohexylmethane diisocyanate and a liquid phase component containing a high boiling point compound.
[0518] The viscosity of the liquid phase componen...
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Abstract
The present invention provides a kind of recovery method, and it is from following general formula (I) (wherein, R 11 It is an organic group with a valence of 1 or more and a valence of 3 or less, and n11 is an integer of 1 to 3) to recover the following general formula (III) (wherein, R 31 A method for a compound represented by an organic group having a valence of 1 or more and a valence of 3 or less, n31 being an integer of 1 to 3), which includes the following steps (1) to (3) or steps (A) and (B) and includes Process (4). Step (1): a step of reacting the above-mentioned liquid-phase component and at least one active hydrogen-containing compound in a reactor. Step (2): A step of returning the condensate obtained by cooling the gas phase components in the reactor to the inside of the reactor. Step (3): A step of discharging gas phase components not condensed in the step (2) to the outside of the reactor. Step (A): a step of mixing the above-mentioned liquid phase component, water, and the compound represented by the above-mentioned general formula (III). Step (B): a step of reacting the above-mentioned liquid-phase component and water in a reactor. Step (4): A step of discharging the reaction liquid containing the compound represented by the above general formula (III) as the liquid phase component in the reactor to the outside of the reactor.
Description
technical field [0001] The present invention relates to a method for recovering active ingredients such as organic amine compounds and aromatic hydroxy compounds from liquid-phase components generated in the production of isocyanates. [0002] This application claims priority based on Japanese Patent Application No. 2017-252607 filed in Japan on December 27, 2017 and Japanese Patent Application No. 2018-014143 filed in Japan on January 30, 2018, the contents of which are incorporated herein by reference. Background technique [0003] Isocyanate compounds having at least one isocyanate group (NCO group) are widely used industrially as raw materials for polyurethanes, polyureas, and the like. [0004] As a method for producing an isocyanate compound, a method using an organic amine compound as a main raw material and phosgene as an auxiliary raw material, and a method using an organic amine compound, carbonate, and urea are known. [0005] In the production methods of these i...
Claims
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Application Information
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