Process for preparing polyphosphonate

• US 3,946,093 A
• Filed: 12/26/1974
• Issued: 03/23/1976
• Est. Priority Date: 04/27/1974
• Status: Expired due to Term

• Current Assignee: Nissan Chemical Industries Limited (Nissan Chemical Corporation)
• Original Assignee: Nissan Chemical Industries Limited (Nissan Chemical Corporation)
• Inventors: Okada, Naotake, Kondo, Keiichi, Koto, Noriaki
• Primary Examiner(s): Raymond, Richard L.
• Application Number:
  US05/536,577
• Time in Patent Office: 453 Days
• Field of Search: 260/973, 260/990
• US Class Current: 558/98
• CPC Class Codes: C08G 79/04 Phosphorus linked to oxygen or to oxygen and carbon

Abstract

An improvement is disclosed in a process for preparing a polyphosphonate which comprises polycondensing an aromatic diol having the formula (I) - (IV) ##SPC1##

wherein Z represents chlorine or bromine atom or a lower alkyl group and m represents 0 or an integer of from 1 to 4 and n represents 0 or an integer of from 1 to 3; Y represents an alkylene group, cycloalkylene group, sulfonyl group, carbonyl group or oxygen atom; with a dihalide or arylphosphonic or thiophosphonic acid having the formula (V) ##SPC2##

wherein A represents oxygen or sulfur atom; X represents chlorine or bromine atom; Z represents chlorine or bromine atom or a lower alkyl group; and 1 represents 0 or an integer of from 1 to 5, wherein the improvement comprises maintaining a solution of the polyphosphonate at a temperature such that solid polyphosphonate is produced after flashing; and then evaporating all or a part of the solvent from the solution by flashing whereby a porous solid polyphosphonate is formed.

Claims

1. In a process for preparing a polyphosphonate which comprises polycondensing an aromatic diol having the formula (I) - (IV) ##SPC5##

wherein Z represents chlorine or bromine atom or a lower alkyl group and m represents 0 or an integer of from 1 to 4 and n represents 0 or an integer of from 1 to 3;

Y represents an alkylene group, cycloalkylene group, sulfonyl group, carbonyl group, or oxygen atom;

with a dihalide of arylphosphonic or thiophosphonic acid having the formula (V) ##SPC6##

wherein A represents oxygen or sulfur atom;

X represents chlorine or bromine atom, and l represents 0 or an integer of from 1 to 5, the improvement which comprises the steps of

1. maintaining in a high pressure zone a solution of said polyphosphonate in an organic solvent at a temperature of 125°

- 300°

C;

2. discharging the solution of step (1) into a low pressure zone wherein all or a portion of the organic solvent is flashed and porous solid polyphosphonate is formed, the pressure of said low pressure zone being lower than the vapor pressure of said organic solvent and lower than that of said high pressure zone; and

3. recovering said porous solid polyphosphonate.

2. The process for preparing a polyphosphonate of claim 1, wherein the molar ratio of the aromatic diol to the dihalide of arylphosphonic or thiophosphonic acid is 1.00:

0.90 - 1.10.

3. The process for preparing a polyphosphonate according to claim 1, wherein an inert gas is fed into the lower pressure zone.

4. The process for preparing a polyphosphonate of claim 1, wherein the solvent for the solution of the polyphosphonate contains less than 500 wt. parts to 100 wt. parts of the polyphosphonate.

5. The process for preparing a polyphosphonate of claim 4, wherein the solvent is selected from the group consisting of chloroform, methylene chloride, 1,2-dichloroethane, 1,1,2-trichloroethane, 1,1,2,2-tetrachloroethane, 1,2-dichloropropane, 1,2-dichlorobutane, chlorobenzene, dichlorobenzene, chlorotoluene, tetrahydrofuran or dimethylformamide.

6. The process for preparing a polyphosphonate of claim 1, wherein the porous solid polyphosphonate is further heated to remove the remaining solvent.

7. The process for preparing a polyphosphonate of claim 1, wherein the higher pressure zone has a pressure of higher than 1 kg/cm² (gauge) and the lower pressure zone has a pressure 1-1000 kg/cm² (gauge) lower than that of the higher pressure zone.

8. The process for preparing a polyphosphonate of claim 1, wherein the solution of the polyphosphonate is heated to a temperature higher than the atmospheric boiling point of the solvent employed.

9. The process for preparing a polyphosphonate of claim 1, wherein the solution of the polyphosphonate is heated to a temperature, such that the solution has enough heat to vapourize all of the solvent in the lower pressure zone.