Flame retardant cellulosic man-made fibers

Patent metadata

Field	Value
Publication number	US-12116701-B2
Application number	US-201816758317-A
Country	US
Kind code	B2
Filing date	Oct 25, 2018
Priority date	Oct 27, 2017
Publication date	Oct 15, 2024
Grant date	Oct 15, 2024

Abstract

A process for the production of an oxidized polymer from a tetrakis hydroxyalkyl phosphonium compound comprising NH 3 or at least one nitrogen compound comprising at least one NH 2 or at least two NH groups, or NH 3 , comprising the steps of: (a) reacting at least one tetrakis hydroxyalkyl phosphonium compound with NH 3 or at least one nitrogen compound in order to obtain a precondensate, wherein the molar ratio of the tetrakis hydroxyakyl phosphonium compound to the nitrogen compound is in the range of 1: (0.05 to 2.0), preferably in the range of 1: (0.5 to 1.5), particularly preferably in the range of 1: (0,65 to 1.2), (b) crosslinking the precondensate obtained in process step (a) with the aid of ammonia to form a crosslinked polymer, (c) oxidizing the crosslinked polymer obtained in step (b) by adding an oxidizing agent to the oxidized polymer, wherein, in step (b), the precondensate from step (a) and the ammonia are each injected by means of a nozzle into a reactor space enclosed by a reactor housing onto a common collision point.

First claim

What is claimed is:

1. A process for the production of an oxidized polymer from a tetrakis hydroxyalkyl phosphonium compound comprising NH 3 or at least one nitrogen compound comprising at least one NH 2 or at least two NH groups, or NH 3 , comprising the steps of:
(a) reacting at least one tetrakis hydroxyalkyl phosphonium compound with NH 3 or at least one nitrogen compound in order to obtain a precondensate, wherein the molar ratio of the tetrakis hydroxyalkyl phosphonium compound to the nitrogen compound in the range of 1:(0.05 to 2.0),
(b) crosslinking the precondensate obtained in process step (a) with the aid of ammonia to form a crosslinked polymer,
(c) oxidizing the crosslinked polymer obtained in step (b) by adding an oxidizing agent to the oxidized polymer wherein,
in step (b), the precondensate from step (a) and the ammonia are each injected by means of a nozzle into a reactor space enclosed by a reactor housing onto a common collision point to form the crosslinked polymer, wherein the crosslinked polymer has a d 99 particle size of less than 1.8 μm.

2. The process according to claim 1 , wherein, in step (b), the precondensate from step (a) and the ammonia are each injected by means of a nozzle into a reactor space enclosed by a reactor housing onto a common collision point, wherein the resulting products are removed from the reactor housing through an opening by means of negative pressure on the product and gas outlet side.

3. The process according to claim 1 , wherein, in step (b), the precondensate from step (a) and the ammonia are each injected by means of a nozzle into a reactor space enclosed by a reactor housing onto a common collision point, wherein a gas, an evaporating liquid, a cooling liquid or a cooling gas is introduced via an opening into the reactor space for maintaining the gas atmosphere in the interior of the reactor, in particular at the collision point of the jets of liquid, or, respectively, for cooling the resulting products, wherein the resulting products and excess gas are removed from the reactor housing through another opening by means of overpressure on the gas inlet side.

4. The process according to claim 1 , wherein the nitrogen compound is selected from the group of urea, thiourea, biuret, melamine, ethylene urea, guanidine and dicyandiamide.

5. The process according to claim 1 , wherein, in step (b), on the one hand, the precondensate and, on the other hand, ammonia are provided as liquid media and sprayed onto the collision point.

6. The process according to claim 5 , wherein, in the case of the precondensate, the liquid medium is an aqueous solution, and, in the case of ammonia, the liquid medium is an aqueous solution.

7. The process according to claim 1 , wherein soluble reaction products are separated after the oxidation according to step (c).

8. The process according to claim 1 , wherein the alkyl radical of the tetrakis hydroxyalkyl phosphonium compound comprises methyl, ethyl, propyl or butyl.

9. The process according to claim 1 , wherein
the molar ratio of the tetrakis hydroxyalkyl phosphonium compound to the nitrogen compound is in the range of 1:(0.5 to 1.5).

10. The process according to claim 9 , wherein
the molar ratio of the tetrakis hydroxyalkyl phosphonium compound to the nitrogen compound is in the range of 1:(0.65 to 1.2).

11. The process according to claim 7 , wherein
the soluble reaction products are separated after the oxidation according to step (c) by means of tangential flow filtration.

Assignees

• Chemiefaser Lenzing Ag

Inventors

• Firgo Heinrich
• Bisjak Clemens

Classifications

• B01F2101/2805

  Mixing plastics, polymer material ingredients, monomers or oligomers · CPC title

• B01F25/23

  Mixing by intersecting jets · CPC title

• D06M2200/30

  Flame or heat resistance, fire retardancy properties · CPC title

• D06M2101/06

  cellulosic · CPC title

• D06M13/322

  with compounds containing nitrogen · CPC title