The invention relates to a method for recovering a diisocyanate that is solid at room temperature from a distillation residue originating from a production process of the diisocyanate, comprising the following steps: (i) mixing the distillation residue with at least one polyisocyanate on the basis of one or more diisocyanates different from the diisocyanate that is solid at room temperature, in such a way that a mixture is obtained that contains 70 to 90 wt. % of the distillation residue and 10 to 30 wt. % of the at least one polyisocyanate, each relative to the mixture, (ii) subjecting the mixture to distillation in a thin-film evaporator and/or a downflow evaporator, thereby obtaining a sump discharge and a gaseous product stream, and (iii) condensing the gaseous product stream and obtaining a solid containing the diisocyanate that is solid at room temperature, the at least one polyisocyanate in step (i) having a residual monomer content of ≤3.0 wt. % as determined by gas chromatography with an internal standard according to EN ISO 10283:2007-11.

The invention relates to a method for recovering a diisocyanate that is solid at room temperature from a distillation residue originating from a production process of the diisocyanate, comprising the following steps: (i) mixing the distillation residue with at least one polyisocyanate on the basis of one or more diisocyanates different from the diisocyanate that is solid at room temperature, in such a way that a mixture is obtained that contains 70 to 90 wt. % of the distillation residue and 10 to 30 wt. % of the at least one polyisocyanate, each relative to the mixture, (ii) subjecting the mixture to distillation in a thin-film evaporator and/or a downflow evaporator, thereby obtaining a sump discharge and a gaseous product stream, and (iii) condensing the gaseous product stream and obtaining a solid containing the diisocyanate that is solid at room temperature, the at least one polyisocyanate in step (i) having a residual monomer content of ≤3.0 wt. % as determined by gas chromatography with an internal standard according to EN ISO 10283:2007-11.

A method is provided for collecting a compound of formula (III) (in which R31 is a monovalent to trivalent organic group and n31 is an integer of 1 to 3) from a liquid phase component that is formed as a by-product in a method for producing a compound of general formula (I) (in which R11 is a monovalent to trivalent organic group and n 11 is an integer of 1 to 3), wherein the collection method contains steps (1) to (3) or steps (A) and (B), and step (4). Step (1): a step for reacting the liquid phase component with at least one active hydrogen-containing compound in a reactor. Step (2): a step for returning a condensed liquid obtained by cooling gas phase components in the reactor to the reactor. Step (3): a step for discharging gas phase components that are not condensed in the step (2) to the outside of the reactor. Step (A): a step for mixing the liquid phase component, water, and a compound of general formula (III). Step (B): a step for reacting the liquid phase component with water inside the reactor. Step (4): a step for discharging, as a liquid phase component inside the reactor, the reaction liquid containing the compound of general formula (III) to the outside of the reactor.
R.sup.11NCO).sub.n11  (I)
R.sup.31NH.sub.2).sub.n31  (III)

A method is provided for collecting a compound of formula (III) (in which R31 is a monovalent to trivalent organic group and n31 is an integer of 1 to 3) from a liquid phase component that is formed as a by-product in a method for producing a compound of general formula (I) (in which R11 is a monovalent to trivalent organic group and n 11 is an integer of 1 to 3), wherein the collection method contains steps (1) to (3) or steps (A) and (B), and step (4). Step (1): a step for reacting the liquid phase component with at least one active hydrogen-containing compound in a reactor. Step (2): a step for returning a condensed liquid obtained by cooling gas phase components in the reactor to the reactor. Step (3): a step for discharging gas phase components that are not condensed in the step (2) to the outside of the reactor. Step (A): a step for mixing the liquid phase component, water, and a compound of general formula (III). Step (B): a step for reacting the liquid phase component with water inside the reactor. Step (4): a step for discharging, as a liquid phase component inside the reactor, the reaction liquid containing the compound of general formula (III) to the outside of the reactor.
R.sup.11NCO).sub.n11  (I)
R.sup.31NH.sub.2).sub.n31  (III)

The invention relates to polyphenyl polymethylene polyisocyanates having an NCO number of at least 29% comprising less than 2% by weight ureas, less than 8% by weight carbodiimides or uretonimines and less than 1000 ppm organic chlorine compounds.

The polyphenyl polymethylene polyisocyanates can be prepared according to the invention by reacting (i) polyphenyl polymethylene polyamines with organic carbonates to give the corresponding polyphenyl polymethylene polycarbamates, (ii) by thermally cleaving the polyphenyl polymethylene polycarbamates to give the polyphenyl polymethylene polyisocyanates,
wherein, prior to the thermal cleavage, the free amino groups or urea groups present in the carhamate crude mixture comprising the polyphenyl polymethylene polycarbamates are reacted with a derivatizing reagent to give amide groups or urethane groups.

The polyphenyl polymethylene polyisocyanates can further be prepared according to the invention, prior to the thermal cleavage, by removing compounds having free amino groups or urea groups present in the carbamate crude mixture from the carbamate crude mixture by filtration of the carbamate crude mixture comprising the polyphenyl polymethylene polycarbamates over a solid acidic adsorbent in the presence of an acid dissolved in the carbamate crude mixture.

The invention relates to polyphenyl polymethylene polyisocyanates having an NCO number of at least 29% comprising less than 2% by weight ureas, less than 8% by weight carbodiimides or uretonimines and less than 1000 ppm organic chlorine compounds.

The polyphenyl polymethylene polyisocyanates can be prepared according to the invention by reacting (i) polyphenyl polymethylene polyamines with organic carbonates to give the corresponding polyphenyl polymethylene polycarbamates, (ii) by thermally cleaving the polyphenyl polymethylene polycarbamates to give the polyphenyl polymethylene polyisocyanates,
wherein, prior to the thermal cleavage, the free amino groups or urea groups present in the carhamate crude mixture comprising the polyphenyl polymethylene polycarbamates are reacted with a derivatizing reagent to give amide groups or urethane groups.

The polyphenyl polymethylene polyisocyanates can further be prepared according to the invention, prior to the thermal cleavage, by removing compounds having free amino groups or urea groups present in the carbamate crude mixture from the carbamate crude mixture by filtration of the carbamate crude mixture comprising the polyphenyl polymethylene polycarbamates over a solid acidic adsorbent in the presence of an acid dissolved in the carbamate crude mixture.

The invention relates to polyphenyl polymethylene polyisocyanates having an NCO number of at least 29% comprising less than 2% by weight ureas, less than 8% by weight carbodiimides or uretonimines and less than 1000 ppm organic chlorine compounds.

The polyphenyl polymethylene polyisocyanates can be prepared according to the invention by reacting (i) polyphenyl polymethylene polyamines with organic carbonates to give the corresponding polyphenyl polymethylene polycarbamates, (ii) by thermally cleaving the polyphenyl polymethylene polycarbamates to give the polyphenyl polymethylene polyisocyanates,
wherein, prior to the thermal cleavage, the free amino groups or urea groups present in the carhamate crude mixture comprising the polyphenyl polymethylene polycarbamates are reacted with a derivatizing reagent to give amide groups or urethane groups.

The polyphenyl polymethylene polyisocyanates can further be prepared according to the invention, prior to the thermal cleavage, by removing compounds having free amino groups or urea groups present in the carbamate crude mixture from the carbamate crude mixture by filtration of the carbamate crude mixture comprising the polyphenyl polymethylene polycarbamates over a solid acidic adsorbent in the presence of an acid dissolved in the carbamate crude mixture.

A method for producing a composition comprising polycarbodiimide, comprising the step of the reaction of a reaction mixture which contains an aromatic polyisocyanate and a carbodiimidising catalyst, wherein, before the reaction, the aromatic polyisocyanate is treated at a temperature of ≧80° C. to ≦150° C. and a pressure of ≧1 mbar to ≦500 mbar by passing through an inert gas and/or during the reaction, the reaction mixture is treated at a temperature of ≧80° C. to ≦150° C. and a pressure of ≧1 mbar to ≦500 mbar by passing through an inert gas and wherein the content of hydrolysable chlorine in the reaction mixture is ≦10 ppm.

The invention relates to a method for producing di- and polyisocyanates of the diphenylmethane series, in which (i) the liquid product flow created in the phosgenation, (ii) the reaction mixture present in an optionally provided reactor for carbamic acid chloride cleaving, (ii) the liquid product flow leaving such an optionally provided reactor for carbamic acid chloride cleaving, (iv) the reaction mixture present in the dephosgenation, or (v) the liquid product flow created in the dephosgenation, is treated with a gaseous hydrogen chloride flow in one stage in a bubble column or in a plate column within a contact time of 1 min to less than 30 min. The product flow treated din this way or in the reaction mixture treated in this way is fed directly (i.e. in particular without further treatment with an inert gas) to the next step of the reaction or workup.

The invention relates to a method for producing di- and polyisocyanates of the diphenylmethane series, in which (i) the liquid product flow created in the phosgenation, (ii) the reaction mixture present in an optionally provided reactor for carbamic acid chloride cleaving, (ii) the liquid product flow leaving such an optionally provided reactor for carbamic acid chloride cleaving, (iv) the reaction mixture present in the dephosgenation, or (v) the liquid product flow created in the dephosgenation, is treated with a gaseous hydrogen chloride flow in one stage in a bubble column or in a plate column within a contact time of 1 min to less than 30 min. The product flow treated din this way or in the reaction mixture treated in this way is fed directly (i.e. in particular without further treatment with an inert gas) to the next step of the reaction or workup.