Granted Patent B2

US 12,637,528 · App. 17/913,449 · Granted May 26, 2026

Inventors: Faissal-Ali El-Toufaili (Ludwigshafen am Rhein, DE); Daniel Barrera-Medrano (Ludwigshafen am Rhein, DE); Dennis Loesch (Ludwigshafen am Rhein, DE); Anna-Corina Schmidt (Trostberg, DE); Kristian Alexander Gill (Ludwigshafen am Rhein, DE); Tobias Joachim Zimmermann (Ludwigshafen am Rhein, DE)

Assignee: BASF SE

C08F220/56B01J13/0065C08F220/06C08F2800/10

Abstract

Claims (65)

1 . Process for making polyacrylamides by polymerizing an aqueous solution comprising at least acrylamide and acrylic acid or salts thereof in the presence of initiators for radical polymerization under adiabatic conditions, wherein the process comprises:

[1] providing an aqueous solution of acrylic acid or salts thereof in at least one pressure-resistant storage tank ( 1 ) having a volume of 10 to 500 m 3 and comprising a heat-insulation layer and means for controlling temperature of the aqueous solution in step [1], wherein a concentration of acrylic acid or their salts is from 2.5 mole/kg to 5 mole/kg relating to a total of the aqueous solution in step [1], and wherein step [1] comprises at least the following sub-steps

[1.1] providing in a transport unit a first liquid chemical product selected from

pure acrylic acid, or

an aqueous solution of acrylic acid or a salt thereof having a concentration of more than 5 mol/kg of acrylic acid relating to a total of the aqueous solution in step [1.1],

[1.2] discharging the first liquid chemical product from the transport unit and diluting it with water in such a manner, that a resultant aqueous solution in step [1.2] has a concentration from 2.5 mole/kg to 5 mole/kg of acrylic acid or salts thereof, relating to the total of the aqueous solution in step [1.2], and

[1.3] transferring said aqueous solution of acrylic acid or salts thereof having a concentration from 2.5 mole/kg to 5 mole/kg of acrylic acid or salts thereof in step [1.2], to the at least one pressure-resistant storage tank ( 1 ), and

[2] providing an aqueous solution of acrylamide in at least one pressure-resistant storage tank ( 2 ) having a volume of 10 to 500 m 3 and comprising a heat-insulation layer, means for controlling temperature of the aqueous solution in step [2], wherein a concentration of the aqueous solution is from 2.5 mole/kg to 5 mole/kg of acrylamide relating to the total of the aqueous acrylamide solution in step [2], and wherein step [2] comprises at least the following sub-steps

[2.1] providing in a transport unit a second liquid chemical product which is an aqueous acrylamide solution having a concentration of more than 5 mol/kg of acrylamide, relating to the total of the aqueous acrylamide solution in step [2.1], and

[2.2] discharging the second liquid chemical product from the transport unit and diluting it with water in such a manner, that a resultant aqueous acrylamide solution has a concentration from 2.5 mole/kg to 5 mole/kg of acrylamide relating to the total of the aqueous acrylamide solution in step [2.2], and

[2.3] transferring said aqueous acrylamide solution in step [2.2] to the at least one pressure-resistant monomer storage tank ( 2 ),

[3] preparing an aqueous monomer mix comprising at least water, acrylamide and partially or fully neutralized acrylic acid in a pressure-resistant mixing vessel ( 3 ) having a volume of 10 to 150 m 3 , comprising a heat-insulation layer and means for controlling temperature of the aqueous monomer mix, wherein step [3] comprises at least the following sub-steps

[3.1] transferring an aqueous solution of acrylic acid or salts thereof from the at least one pressure-resistant storage tank ( 1 ) into the pressure-resistant mixing vessel ( 3 ),

[3.2] transferring an aqueous solution of acrylamide from the at least one pressure-resistant storage tank ( 2 ) into the pressure-resistant mixing vessel ( 3 ),

[3.3] adding an aqueous base into the pressure-resistant mixing vessel, while mixing components in the pressure-resistant mixing vessel ( 3 ) and controlling temperature of the mixture in the vessel ( 3 ) to maintain a temperature of not more than 40° C.,

wherein an amount of all monomers in the aqueous monomer mix is at least 2 moles/kg, relating to the total of all components of the aqueous monomer mix, and

[4] transferring the aqueous monomer mix prepared in course of step [3] to a pressure-resistant polymerization unit ( 5 ) having a volume of 10 to 150 m 3 , adding initiators for radical polymerization and polymerizing the aqueous monomer mix under adiabatic conditions, thereby obtaining an aqueous polyacrylamide gel.

2 . Process according to claim 1 , wherein

the pressure-resistant storage tank ( 1 ) has a design pressure of at least 4 bar gauge,

the pressure-resistant storage tank ( 2 ) has a design pressure of at least 4 bar gauge,

the pressure-resistant mixing vessel ( 3 ) has a volume of 10 to 50 m 3 and a design pressure of at least 8 bar gauge, and

the pressure-resistant polymerization unit ( 5 ) has a design pressure of at least 4 bar gauge.

3 . Process according to claim 1 , wherein steps [1.2] and [2.2] are carried out by continuously mixing a flow of the respective liquid chemical product with a flow of water, thereby obtaining a flow of an aqueous monomer solution of acrylic acid or salt thereof in step [1.2] and aqueous monomer solution of acrylamide in step [2.2] which is filled into the respective pressure-resistant monomer storage tank.

4 . Process according to claim 1 , wherein steps [1.2] and [2.2] are carried out by

discharging the respective liquid chemical product from the transport unit by means of a pump and pumping a flow of the respective liquid chemical product through a pipe to a mixing unit ( 4 a ) or ( 4 b ), wherein the pipe is equipped with a flow meter for controlling the flow and a valve for adjusting the flow,

discharging water from a water storage tank by means of a pump and pumping a flow of water through a pipe to the mixing unit, wherein the pipe is equipped with a flow meter for controlling the flow of water and a valve for adjusting the flow,

mixing the flow of water with the flow of the respective liquid chemical product in the mixing unit,

adjusting the flow of water and the flow of the respective liquid chemical product by means of the valves, thereby adjusting the concentration of monomer of the respective liquid chemical product to the desired value in the range from 2.5 mole/kg to 5 mole/kg, and

transferring the resultant monomer solution to the respective pressure-resistant monomer storage tank.

5 . Process according to claim 4 , wherein the mixing unit comprises at least a T-fitting connecting the water pipe and a monomer pipe and a further pipe which is connected to the respective pressure-resistant monomer storage tank.

6 . Process according to claim 5 , wherein the mixing unit additionally comprises a static mixer.

7 . Process according to claim 1 , wherein temperature of the aqueous solution of acrylic acid or salts thereof in the at least one pressure-resistant storage tank ( 1 ) and the aqueous solution of acrylamide in the at least one pressure-resistant storage tank ( 2 ) is maintained at ≤25° C.

8 . Process according to claim 1 , wherein a temperature of the aqueous monomer mix-in the pressure-resistant mixing vessel is maintained at ≤5° C.

9 . Process according to claim 1 , wherein the first liquid chemical product is pure acrylic acid or an aqueous solution of acrylic acid, and in step [3.3] an aqueous base is added into the pressure-resistant mixing vessel.

10 . Process according to claim 1 , wherein the concentration of all monomers in the aqueous monomer mix for polymerization is from 2.75 to 4.5 mole/kg, relating to the total of all components of the aqueous monomer mix.

11 . Process according to claim 1 , wherein the pressure-resistant polymerization unit has a volume from 10 to 40 m 3 .

12 . Process according to claim 1 , wherein the pressure-resistant polymerization unit comprises a cylindrical upper part, a conical part at its lower end, feeds for the aqueous monomer mix and a bottom opening for removing the polyacrylamide gel.

13 . Process according to claim 1 , wherein the process comprises additionally the following process steps:

[5] removing the aqueous polyacrylamide gel from the polymerization unit, and

[6] comminuting the aqueous polyacrylamide gel and mixing it with an aqueous liquid, thereby obtaining an aqueous polyacrylamide composition having a concentration of 0.01 to 14.9% by weight of polyacrylamides, relating to the total of all components of the aqueous polyacrylamide composition in step [6].

14 . Process according to claim 13 , wherein the process comprises additionally the following steps:

[7] transporting the aqueous polyacrylamide composition in a transport unit having a volume from 1 m 3 to 40 m 3 by transport means selected from the group of trucks, railcars or ships from a manufacturing site (location A) to a different location B, and

[8] removing the aqueous polyacrylamide composition from the transport unit in step [7] at the location B.

15 . Process according to claim 13 , wherein the concentration of the polyacrylamides in the aqueous polyacrylamide composition is from 3.1 wt. % to 7 wt. %, relating to the total of all components of the aqueous composition in step [6].

16 . Process according to claim 1 , wherein the pressure-resistant polymerization unit is a transportable pressure-resistant polymerization unit, and the process comprises additionally the following process steps:

[5a] transporting the pressure-resistant polymerization unit filled with the aqueous polyacrylamide gel from the manufacturing site (location A) to a different location B,

[6a] removing the aqueous polyacrylamide gel from the transportable pressure-resistant polymerization unit at the location B,

[7a] comminuting and dissolving the aqueous polyacrylamide gel in an aqueous liquid at the location B, thereby obtaining an aqueous polyacrylamide composition having a concentration of 0.01 to 14.9% by weight of polyacrylamides, relating to the total of all components of the aqueous polyacrylamide composition.

17 . Process according to claim 1 , wherein the pressure resistant storage tanks ( 1 ) and ( 2 ) have a volume from 10 to 200 m 3 each.

18 . Process according to claim 17 , wherein the process is carried out in a modular, relocatable plant.

19 . Process according to claim 1 , wherein

the pressure-resistant storage tank ( 1 ) has a design pressure of 6 bar to 8 bar gauge, and the concentration of the aqueous solution of acrylic acid or salts thereof in said pressure-resistant storage tank ( 1 ) is from 4.5 to 5 mole/kg,

the pressure-resistant storage tank ( 2 ) has a design pressure of 6 to 8 bar gauge, and the concentration of the aqueous solution of acrylamide in said pressure-resistant storage tank ( 2 ) is from 4.5 to 5 mole/kg,

the pressure-resistant mixing vessel ( 3 ) has a design pressure of 15 to 20 bar gauge, and

the pressure-resistant polymerization unit ( 5 ) has a design pressure of 15 to 20 bar gauge.

20 . Process according to claim 1 , wherein

the pressure-resistant storage tank ( 1 ) has a design pressure of 3 bar to 4 bar gauge, and the concentration of the aqueous solution of acrylic acid or salts thereof in said pressure-resistant storage tank ( 1 ) is from 3.5 to 4.2 mole/kg,

the pressure-resistant storage tank ( 2 ) has a design pressure of 3 to 4 bar gauge, and the concentration of the aqueous solution of acrylamide in said pressure-resistant storage tank ( 2 ) is from 3.5 to 4.2 mole/kg,

the pressure-resistant mixing vessel ( 3 ) has a design pressure of 11 to 15 bar gauge, and

the pressure-resistant polymerization unit ( 5 ) has a design pressure of 11 to 15 bar gauge.

21 . Process according to claim 1 , wherein,

the at least one pressure-resistant storage tank ( 1 ) has a design pressure of 2 bar to 3 bar gauge, and the concentration of the aqueous solution of acrylic acid or salts thereof in said pressure-resistant storage tank ( 1 ) is from 3.5 to 4.2 mole/kg,

the at least one pressure-resistant storage tank ( 2 ) has a design pressure of 2 to 3 bar gauge, and the concentration of the aqueous solution of acrylamide in said pressure-resistant storage tank ( 2 ) is from 3.5 to 4.2 mole/kg,

the pressure-resistant mixing vessel ( 3 ) has a design pressure of 7 to 10 bar gauge, and

the pressure-resistant polymerization unit ( 5 ) has a design pressure of 7 to 10 bar gauge.

Assignments (3)

Priority Claims (1)

Continuity (1)

References Cited (31)