Patent US4603193A successfully refreshed from Google Patents.
US4603193A
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Polycondensation process with aerosol mist of aqueous solution of reactant salts
Assignee: Syensqo Specialty Polymers USA LLC
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Filing: 1984-02-23
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Granted: 1986-07-29
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Expires: 2004-02-23
Abstract
Abstract A process for the manufacture of polyamides, polyamide-imides and polyimides which process comprises preparing a salt of an aliphatic or aromatic diamine or a mixture of these and di, tri or tetracarboxylic acid or mixture of these or their corresponding anhydride by reacting both feedstocks at a temperature of about 300 DEG to 500 DEG F. in a solvent medium provided the water content of the resulting solution is below 25% water by weight the resulting salt solution is subjected to a pressure of about 1500-3000 psig and is then passed through a preheat zone where the temperature is increased to about 625 DEG F., the total residence time is kept at about 25 to about 50 seconds. The reactants are flashed through a control valve or nozzle to give an aerosol mist at a pressure of about 0-400 psig, the polymerization is further carried out in a flash reactor with a high heat flux and with wall temperatures of about 600 DEG F. to about 1000 DEG F. and melt temperatures of about 500 DEG F. to about 750 DEG F., the total polymer residence time in the reactor is kept about 0.1 to about 20 seconds. The novel compositions are useful for engineering resins. Also a process for the manufacture of polyesters, polycarbonates, polyarylates and polyesterarylates by the process disclosed above, except that instead of a salt a prepolymer is prepared and the reactants for polyesters are dicarboxylic acids and glycols, for polycarbonates, diphenols and phosgene, for polyarylates, diphenols and dicarboxylic acids and for polyesterarylates, dicarboxylic acids and phosgene.
Inventors
- 👤 Joel A. Richardson
- 👤 Wassily Poppe
- 👤 Benjamin A. Bolton
- 👤 Edward E. Paschke
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 13:53
CPC Classifications
C; C08; C08G; C08G73/00; C08G73/06; C08G73/10; C08G73/14; C08G63/00; C08G63/78; C08G69/00; C08G69/02; C08G69/26; C08G69/28; C08G73/1003; C08G73/1007; C08G73/1028
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
191 words
A process for manufacture of polyamide-imide which process comprises combining components comprising metaphenylene diamine, trimellitic anhydride and isophthalic acid in a mole ratio of about 100:10:90 to 100:50:50 and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising salts of metaphenylene diamine and trimellitic anhydride and of metaphenylene diamine and isophthalic acid, provided the solvent content of the solution is below 25% by weight, pressurizing the solution to about 1500 to about 3000 psig, passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F. during a residence time in the preheat zone of about 25 to about 50 seconds, flashing said solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salts, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 2
Dependent Claim
191 words
A process for manufacture of polyamide-imide which process comprises combining components comprising metaphenylene diamine, trimellitic anhydride and isophthalic acid in a mole ratio of about 100:10:90 to 100:50:50 and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising salts of metaphenylene diamine and trimellitic anhydride and of metaphenylene diamine and isophthalic acid, provided the solvent content of the solution is below 25% by weight, pressurizing the solution to about 1500 to about 3000 psig, passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F. during a residence time in the preheat zone of about 25 to about 50 seconds, flashing said solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salts, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 3
Dependent Claim
10 words
The process of claim 1 wherein said solvent is water.
Claim 4
Dependent Claim
88 words
A process for manufacture of polyamide-imide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one tricarboxylic acid or an anhydride thereof and at least one diamine at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1,000° F. for about 0.1 second to about 20 seconds to produce the polyamide-imide.
Claim 5
Dependent Claim
88 words
A process for manufacture of polyamide-imide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one tricarboxylic acid or an anhydride thereof and at least one diamine at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1,000° F. for about 0.1 second to about 20 seconds to produce the polyamide-imide.
Claim 6
Dependent Claim
10 words
The process of claim 3 wherein said solvent is water.
Claim 7
Dependent Claim
35 words
The process of claim 3 wherein said diamine is selected from the group consisting of methylenebis(aniline), hexamethylene diamine, meta-phenylene diamine, and oxybis(aniline), and said tricarboxylic acid is trimellitic acid, and said anhydride is trimellitic anhydride.
Claim 8
Dependent Claim
198 words
A process for manufacture of polyimide which process comprises combining components comprising an aliphatic or aromatic diamine or a mixture of these, at least one tetracarboxylic acid or an anhydride thereof and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F. during a residence time in the preheat zone of about 25 to about 50 seconds, flashing said solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1,000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 9
Dependent Claim
198 words
A process for manufacture of polyimide which process comprises combining components comprising an aliphatic or aromatic diamine or a mixture of these, at least one tetracarboxylic acid or an anhydride thereof and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F. during a residence time in the preheat zone of about 25 to about 50 seconds, flashing said solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1,000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 10
Dependent Claim
11 words
The process of claim 6 wherein said solvent medium is water.
Claim 11
Dependent Claim
89 words
A process for manufacture of polyimide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one tetracarboxylic acid or an anhydride thereof and at least one diamine at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1,000° F. for about 0.1 second to about 20 seconds to produce the polyimide.
Claim 12
Dependent Claim
89 words
A process for manufacture of polyimide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one tetracarboxylic acid or an anhydride thereof and at least one diamine at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1,000° F. for about 0.1 second to about 20 seconds to produce the polyimide.
Claim 13
Dependent Claim
200 words
A process for the manufacture of a polyamideimide which process comprises combining components comprising an aliphatic or aromatic diamine or a mixture of these, at least one tricarboxylic acid or an anhydride thereof, and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and the acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F., maintaining the solution in the preheat zone for about 25 to about 50 seconds, flashing the solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 14
Dependent Claim
200 words
A process for the manufacture of a polyamideimide which process comprises combining components comprising an aliphatic or aromatic diamine or a mixture of these, at least one tricarboxylic acid or an anhydride thereof, and aqueous solvent at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and the acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F., maintaining the solution in the preheat zone for about 25 to about 50 seconds, flashing the solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 15
Dependent Claim
10 words
The process of claim 9 wherein said solvent is water.
Claim 16
Dependent Claim
34 words
The process of claim 9 wherein said diamine is selected from the group consisting of hexamethylene diamine, methylenebis(aniline), meta-phenylene diamine, and oxybis(aniline), said tricarboxylic acid is trimellitic acid and said anhydride is trimellitic anhydride.
Claim 17
Dependent Claim
10 words
The process of claim 9 wherein the process is continuous.
Claim 18
Dependent Claim
224 words
A process for the manufacture of a polyamideimide or polyimide which process comprises combining components comprising aqueous solvent, an aliphatic or aromatic diamine or a mixture of these, and, in the case of polyamide-imide manufacture, at least one tricarboxylic acid or an anhydride thereof or, in the case of polyimide manufacture, at least one tetracarboxylic acid or an anhydride thereof, at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and the acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F., maintaining the solution in the preheat zone for about 25 to about 50 seconds, flashing the solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 19
Dependent Claim
224 words
A process for the manufacture of a polyamideimide or polyimide which process comprises combining components comprising aqueous solvent, an aliphatic or aromatic diamine or a mixture of these, and, in the case of polyamide-imide manufacture, at least one tricarboxylic acid or an anhydride thereof or, in the case of polyimide manufacture, at least one tetracarboxylic acid or an anhydride thereof, at a temperature of about 300° F. to about 500° F. to form a solution comprising a salt of the diamine or mixture thereof and the acid or anhydride, provided the solvent content of the solution is below 25% by weight, pressurizing said solution to a pressure of about 1500 to about 3000 psig and then passing said solution through a preheat zone where the temperature of said solution is increased to between about 550° F. and about 625° F., maintaining the solution in the preheat zone for about 25 to about 50 seconds, flashing the solution through a control means at a pressure of about 0 to about 400 psig to give an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor with wall temperatures of about 600° F. to about 1000° F., and maintaining a total residence time of said reactants in the reactor at about 0.1 second to about 20 seconds.
Claim 20
Dependent Claim
115 words
A process for manufacture of polyamide-imide or polyimide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one diamine and, in the case of polyamide-imide manufacture, at least one tricarboxylic acid or an anhydride thereof, or in the case of polyimide manufacture, at least one tetracarboxylic acid or an anhydride thereof, at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1000° F. for about 0.1 second to about 20 seconds to produce the polyamide-imide or polyimide.
Claim 21
Dependent Claim
115 words
A process for manufacture of polyamide-imide or polyimide comprising atomizing components comprising an aqueous solution of salt obtained from feed materials comprising at least one diamine and, in the case of polyamide-imide manufacture, at least one tricarboxylic acid or an anhydride thereof, or in the case of polyimide manufacture, at least one tetracarboxylic acid or an anhydride thereof, at a pressure of about 0 to about 400 psig to form an aerosol mist of reactants comprising said salt, polymerizing said reactants while passing said aerosol mist through a flash reactor having wall temperatures of about 400° F. to about 1000° F. for about 0.1 second to about 20 seconds to produce the polyamide-imide or polyimide.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-07-28 | 1990-01-27 | 1990-07-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-07-28 | 1994-01-27 | 1994-07-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-07-28 | 1998-01-27 | 1998-07-29 | $7700.00 | Window Closed / Lapsed |