US4071479A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Reclamation processing of vinyl chloride polymer containing materials and products produced thereby
Assignee: AT&T Inc
•
Filing: 1976-03-25
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Granted: 1978-01-31
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Expires: 1996-03-25
Abstract
Abstract Recompoundable polyvinyl chloride suitable to be recompounded for reuse, for example, in cable and wire production is recovered from a scrap material which includes plasticized polyvinyl chloride. A charge of plasticized polyvinyl chloride scrap material is treated with a solvent such as methyl ethyl ketone, tetrahydrofuran, cyclohexanone or dimethyl formamide to form a solvent mixture with one component thereof being a solvent solution of dissolved vinyl chloride polymer and plasticizers. The mixture is heated and agitated and scrap metal and other gross solids, if present, are removed. Then the solvent mixture is treated with an acid which advantageously causes a flocculation of suspended insolubles such as pigments and fillers. Except when using cyclohexanone as the solvent, the treatment with the acid must be accomplished, unexpectedly, in the presence of an additional flocculating agent such as a cellulose acetate which is soluble in the solution and which is insolubilized by the acid on refluxing. Recompoundable polyvinyl chloride is precipitated out by a non-solvent for the polyvinyl chloride which is miscible with the solvent in substantially all proportions, which will dissolve the plasticizer. The solvent and the non-solvent are removed from the plasticizer and are recovered separately by fractional distillation, for example.
Inventors
- 👤 Barret Broyde
- 👤 Judith Archer Delles
- 👤 Steven Forrest North
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 04:45
CPC Classifications
C; C08; C08J; C08J11/00; C08J11/04; C08J11/06; C08J11/08; C08J2327/00; C08J2327/02; C08J2327/04; C08J2327/06; Y; Y02; Y02W; Y02W30/00; Y02W30/50; Y02W30/62
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
149 words
A process for recovering a reusable essentially pure vinyl chloride polymer resin from a polymer mixture which comprises plasticized polyvinyl chloride and insoluble particulate additives, which includes the steps of: contacting a polymer mixture which comprises plasticized polyvinyl chloride and insoluble particulate additives with a solvent for vinyl chloride polymers to form a solvent mixture comprising a solvent solution of dissolved vinyl chloride polymer and plasticizers and insoluble particulate additives in suspension; treating the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent to flocculate and remove the suspended particulate additives; and treating the solvent solution with a non-solvent which is miscible with the solvent in substantially all proportions and which is a solvent for the plasticizer to precipitate an essentially pure vinyl chloride polymer resin therefrom.
Claim 2
Dependent Claim
149 words
A process for recovering a reusable essentially pure vinyl chloride polymer resin from a polymer mixture which comprises plasticized polyvinyl chloride and insoluble particulate additives, which includes the steps of: contacting a polymer mixture which comprises plasticized polyvinyl chloride and insoluble particulate additives with a solvent for vinyl chloride polymers to form a solvent mixture comprising a solvent solution of dissolved vinyl chloride polymer and plasticizers and insoluble particulate additives in suspension; treating the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent to flocculate and remove the suspended particulate additives; and treating the solvent solution with a non-solvent which is miscible with the solvent in substantially all proportions and which is a solvent for the plasticizer to precipitate an essentially pure vinyl chloride polymer resin therefrom.
Claim 3
Dependent Claim
25 words
The process of claim 1, which also includes the step of contacting the solvent mixture with calcium hydroxide subsequent to the treatment with the acid.
Claim 4
Dependent Claim
76 words
The process of claim 1, wherein the polymer mixture is a scrap conductor material and the solvent is a solvent selected from the group consisting of methyl ethyl ketone, tetrahydrofuran, and dimethyl formamide, and the step of treating the solvent mixture to flocculate and remove the suspended particulates includes treating the solvent mixture with the acid in the presence of a flocculating agent which is soluble in the solvent solution and insolubilized by acid on refluxing.
Claim 5
Dependent Claim
72 words
The process of claim 1 wherein the polymer mixture is a scrap plastic scrap material, the solvent is selected from the group consisting of methyl ethyl ketone, tetrahydrofuran, and dimethyl formamide and the step of treating the solvent mixture to flocculate and remove the suspended particulates includes the addition of a flocculating agent to the solvent mixture prior to the addition of the acid and the flocculating agent is a cellulose acetate.
Claim 6
Dependent Claim
24 words
The process of claim 1, wherein the acid is an acid selected from the group consisting of nitric acid, sulfuric acid, and hydrochloric acid.
Claim 7
Dependent Claim
23 words
The process of claim 1, wherein the solvent is selected from the group consisting of tetrahydrofuran, methyl ethyl ketone, cyclohexanone, or dimethyl formamide.
Claim 8
Dependent Claim
27 words
The process of claim 1, wherein the non-solvent is selected from the group consisting of methanol, isopropanol, n-butanol, or an azeotrope of methyl ethyl ketone and methanol.
Claim 9
Dependent Claim
29 words
The process of claim 1, which subsequent to the step of contacting the polymer mixture with the solvent includes the step of removing gross solids from the solvent mixture.
Claim 10
Dependent Claim
69 words
The process of claim 1, wherein the non-solvent for the vinyl chloride polymer produces fine-grained unagglomerated vinyl chloride particles, the non-solvent being miscible in all proportions with the solvent for the vinyl chloride, the non-solvent for the vinyl chloride being a solvent for the plasticizer in the plasticized polyvinyl chloride and having a boiling point significantly different from both the plasticizer and the solvent for the vinyl chloride polymer.
Claim 11
Dependent Claim
21 words
The process of claim 1, wherein the weight percent vinyl chloride resin dissolved in the solvent is at least one-half percent.
Claim 12
Dependent Claim
38 words
The method of claim 1, wherein the plasticized vinyl chloride polymer includes substantially a single plasticizing constituent, and the plasticizer recovery step comprises removing the plasticizer remaining behind after distilling the solution comprising the solvent, non-solvent and plasticizers.
Claim 13
Dependent Claim
35 words
The process pursuant to claim 1, wherein the plasticized vinyl chloride polymer includes more than one plasticizing constituent each with different boiling points, and the plasticizing constituents are separated from one another by fractional distillation.
Claim 14
Independent Claim
232 words
A method of separating metal, polyvinyl chloride and plasticizer from scrap conductor scrap material and plasticized polyvinyl chloride which also includes insoluble particulate matter comprising pigments and fillers, comprising the steps of: dissolving the polyvinyl chloride in methyl ethyl ketone at a temperature above ambient to form a solvent mixture containing a solvent solution comprising dissolved polyvinyl chloride, entrained particulate material and undissolved conductor metal; separating the undissolved metal from the solvent mixture; treating the solvent mixture with an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent in the presence of a cellulose acetate flocculating agent which is soluble in the solvent solution and is insolubilized by an acid on reflux to cause a flocculation of the pigments and fillers; treating the solvent solution to precipitate out the polyvinyl chloride by adding methanol in which the polyvinyl chloride is substantially insoluble and which produces fine-grained unagglomerated polyvinyl chloride particles, the methanol being mixcible in all proportions with the methyl ethyl ketone, being a solvent for the plasticizer in the resin material, and having itself a boiling point significantly different from both the methyl ethyl ketone and the plasticizer; removing the polyvinyl chloride; and fractionating the remaining solvent solution to recover separately the solvent, an azeotrope of the methanol and methyl ethyl ketone and the plasticizer.
Claim 15
Independent Claim
232 words
A method of separating metal, polyvinyl chloride and plasticizer from scrap conductor scrap material and plasticized polyvinyl chloride which also includes insoluble particulate matter comprising pigments and fillers, comprising the steps of: dissolving the polyvinyl chloride in methyl ethyl ketone at a temperature above ambient to form a solvent mixture containing a solvent solution comprising dissolved polyvinyl chloride, entrained particulate material and undissolved conductor metal; separating the undissolved metal from the solvent mixture; treating the solvent mixture with an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent in the presence of a cellulose acetate flocculating agent which is soluble in the solvent solution and is insolubilized by an acid on reflux to cause a flocculation of the pigments and fillers; treating the solvent solution to precipitate out the polyvinyl chloride by adding methanol in which the polyvinyl chloride is substantially insoluble and which produces fine-grained unagglomerated polyvinyl chloride particles, the methanol being mixcible in all proportions with the methyl ethyl ketone, being a solvent for the plasticizer in the resin material, and having itself a boiling point significantly different from both the methyl ethyl ketone and the plasticizer; removing the polyvinyl chloride; and fractionating the remaining solvent solution to recover separately the solvent, an azeotrope of the methanol and methyl ethyl ketone and the plasticizer.
Claim 16
Independent Claim
87 words
A method of separating fillers, metal salts, and insoluble pigments from a vinyl chloride polymer scrap material, which includes: contacting a vinyl chloride polymer scrap material with a solvent which is a solvent for vinyl chloride polymer and plasticizers to form a solvent mixture; and contacting the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent to flocculate the fillers, metal salts and insoluble pigments.
Claim 17
Independent Claim
87 words
A method of separating fillers, metal salts, and insoluble pigments from a vinyl chloride polymer scrap material, which includes: contacting a vinyl chloride polymer scrap material with a solvent which is a solvent for vinyl chloride polymer and plasticizers to form a solvent mixture; and contacting the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent to flocculate the fillers, metal salts and insoluble pigments.
Claim 18
Dependent Claim
22 words
The method of claim 14, wherein the acid is selected from the group consisting of nitric acid, sulfric acid, and hydrochloric acid.
Claim 19
Dependent Claim
21 words
The method of claim 14, which also includes the step of adding calcium hydroxide subsequent to the addition of the acid.
Claim 20
Dependent Claim
33 words
The method of claim 14, wherein the solvent includes methyl ethyl ketone, tetrahydrofuran and dimethyl formamide and the method further includes the addition of cellulose acetate prior to the addition of the acid.
Claim 21
Dependent Claim
33 words
The method of claim 14, wherein the solvent is selected from the group consisting of tetrahydrofuran, methyl ethyl ketone, cyclohexanone or dimethyl formamide and the scrap material is a scrap conductor scrap material.
Claim 22
Dependent Claim
20 words
The method of claim 14, wherein the solvent is cyclohexanone and the scrap material is a scrap plastic scrap material.
Claim 23
Independent Claim
97 words
A method of recovering an essentially pure plasticized polyvinyl chloride resin from a polyvinyl chloride scrap material, which includes the step of: contacting a polyvinyl chloride scrap material with a solvent which is a solvent for a vinyl chloride polymer and plasticizers to form a solvent mixture; flocculating out insoluble additives by treating the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent; and evaporating the solvent to recover an essentially pure plasticized polyvinyl chloride.
Claim 24
Independent Claim
97 words
A method of recovering an essentially pure plasticized polyvinyl chloride resin from a polyvinyl chloride scrap material, which includes the step of: contacting a polyvinyl chloride scrap material with a solvent which is a solvent for a vinyl chloride polymer and plasticizers to form a solvent mixture; flocculating out insoluble additives by treating the solvent mixture with at least an acid which is selected from the group consisting of an inorganic acid and an inorganic acid solution and which is substantially soluble in the solvent; and evaporating the solvent to recover an essentially pure plasticized polyvinyl chloride.
Claim 25
Dependent Claim
22 words
The method of claim 20, wherein the acid is selected from the group consisting of nitric acid, sulfuric acid, and hydrochloric acid.
Claim 26
Dependent Claim
19 words
The method of claim 20, which also includes the addition of calcium hydroxide after the addition of the acid.
Claim 27
Dependent Claim
43 words
The method of claim 20 wherein the solvent includes methyl ethyl ketone, tetrahydrofuran or dimethyl formamide and the method also includes the addition of a flocculating agent which is soluble in the solvent solution and which is insolubilized by an acid or reflux.
Claim 28
Dependent Claim
23 words
The method of claim 20, wherein the solvent is selected from the group consisting of tetrahydrofuran, methyl ethyl ketone, cyclohexanone or dimethyl formamide.
Claim 29
Dependent Claim
20 words
An essentially pure polyvinyl chloride resin recovered from a scrap plastic charge in accordance with the method of claim 1.
Claim 30
Dependent Claim
21 words
An essentially pure plasticized polyvinyl chloride resin recovered from a scrap plastic charge in accordance with the method of claim 14.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1981-01-30 | 1981-08-01 | 1982-01-31 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-01-30 | 1985-08-01 | 1986-01-31 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-01-30 | 1989-08-01 | 1990-01-31 | $7700.00 | Window Closed / Lapsed |