Reaction #1379904

Reaction equation

Pionin

sodium hydroxide

ethylenediamine tetraacetate tetrasodium salt

styrene

acrylic acid

tert-dodecyl mercaptan

sodium hydroxide

ammonium hydroxide

→

RP-1

Solvents

water

Conditions

Workup

1. 1
   OtherTo a polymerization vessel of a gas monomer reaction apparatus (manufactured by Taiatsu Techno Corporation, TAS-2J type)
2. 2
   OtherDegassing
3. 3
   Otheris elevated to 60° C
4. 4
   workup.ADDITIONThereto was added a solution of 1.875 g of ammonium persulfate
5. 5
   workup.DISSOLUTIONdissolved in 50 mL of water
6. 6
   workup.STIRRINGthe mixture was stirred for 5 hours as it
7. 7
   Otherwas further elevated to 90° C.
8. 8
   workup.STIRRINGby stirring for 3 hours
9. 9
   Otherthe reaction
10. 10
    Otherto reach to the room temperature
11. 11
    workup.ADDITIONthe mixture was treated
12. 12
    Otherto give the molar ratio of Na+ ion
13. 13
    FiltrationThereafter, filtration with a polypropylene
14. 14
    Filtrationfilter
15. 15
    Otherto remove foreign substances such as dust

Procedure

To a polymerization vessel of a gas monomer reaction apparatus (manufactured by Taiatsu Techno Corporation, TAS-2J type) were charged 287 g of distilled water, 7.73 g of a surfactant (Pionin A43-S (manufactured by TAKEMOTO OIL & FAT CO., LTD.): solid matter content of 48.5% by weight), 14.06 mL of 1 mol/L sodium hydroxide, 0.15 g of ethylenediamine tetraacetate tetrasodium salt, 255 g of styrene, 11.25 g of acrylic acid, and 3.0 g of tert-dodecyl mercaptan, followed by sealing of the reaction vessel and stirring at a stirring rate of 200 rpm. Degassing was conducted with a vacuum pump, followed by repeating nitrogen gas replacement several times. Thereto was injected 108.75 g of 1,3-butadiene, and the inner temperature is elevated to 60° C. Thereto was added a solution of 1.875 g of ammonium persulfate dissolved in 50 mL of water, and the mixture was stirred for 5 hours as it stands. The temperature was further elevated to 90° C., followed by stirring for 3 hours. After completing the reaction, the inner temperature was lowered to reach to the room temperature, and thereafter the mixture was treated by adding 1 mol/L sodium hydroxide and ammonium hydroxide to give the molar ratio of Na+ ion:NH4+ ion=1:5.3, and thus, the pH of the mixture was adjusted to 8.05. Thereafter, filtration with a polypropylene filter having the pore size of 1.0 μm was conducted to remove foreign substances such as dust followed by storage. Accordingly, Compound No. RP-1 was obtained in an amount of 774.7 g. Upon the measurement of halogen ion by ion chromatography, concentration of chloride ion was revealed to be 3 ppm. As a result of the measurement of the concentration of the chelating agent by high performance liquid chromatography, it was revealed to be 145 ppm.

Source