# US 5,702,609 A · Water retrieval from aqueous mixture of organic phosphates

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- Number: US 5,702,609 A
- Document ID: US5702609A
- Status: Granted
- Kind: A
- Application number: 08/410,983
- Filed: 1995-03-27
- Granted: 1997-12-30
- Earliest claimed: 1995-03-27
- Assignees: Niagara Mohawk Power Corporation
- Inventors: Carey M. Merritt
- Web page: https://patentgrep.com/patent/US5702609A

## CPC

- C02F 9/00: Multistage treatment of water, waste water or sewage
- C02F 1/285: {using synthetic organic sorbents}
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)

## Abstract

Process and apparatus for separating aryl phosphates and esters and hydrolysates thereof from water in an aqueous mixture thereof. A superposed layer of the mixture is decanted from a lower layer of the phosphates, esters and hydrolysates. The superposed layer is filtered with a filter having a pore size of between 1 micron and 25 microns to remove globules and solid particles. The effluent is then subjected to demineralization with an anion exchange resin to remove most of the hydrolysates. Thereafter a sorber composed of an organic polymeric material such as polypropylene removes any remaining phosphates and esters down to less than 250 ppb.

## Claims

### Claim 1

The process of separating aryl phosphates and esters and hydrolysates thereof from water in an aqueous mixture thereof comprising,
forming a superposed layer from said mixture of said phosphates, esters and hydrolysates, and water and a lower layer of primarily said esters and phosphates,
removing said lower layer of said esters and phosphates to isolate said upper or superposed layer of said mixture, filtering said layer of said mixture with a filter having a pore size of between 1 micron to about 25 microns,
subjecting the effluent from said filtering to demineralization with an anion exchange resin,
thereafter subjecting the effluent from said demineralization to a sorber composed of organic polymeric material to produce an effluent consisting essentially of water substantially without said phosphates, esters or hydrolysates thereof.

### Claim 2 (depends on 1)

The process of claim 1 including,
removing solid particles and liquid globules of said phosphates and esters with said filtering.

### Claim 3 (depends on 1)

The process of claim 1 including,
removing hydrolysates of said phosphates and esters with said anion exchange resin.

### Claim 4 (depends on 3)

The process of claim 3 including,
said removing of hydrolysates with said anion exchange resin being the substantial majority of the hydrolysates present.

### Claim 5 (depends on 1)

The process of claim 1 including,
removing remaining amounts of said phosphates, esters and said hydrolysates by said sorption.

### Claim 6 (depends on 1)

The process of claim 1 including,
separating said lower and upper layers by decanting.

### Claim 7 (depends on 1)

The process of claim 1 including,
said filter for said filtering step having a pore size ranging from 5-10 microns.

### Claim 8 (depends on 1)

The process of claim 1 including,
said filter being composed of polypropylene.

### Claim 9 (depends on 1)

The process of claim 1 including,
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines.

### Claim 10 (depends on 1)

The process of claim 1 including,
removing at least 90% of the hydrolysates present in said mixture and substantially none of the phosphates or esters by means of said demineralization.

### Claim 11 (depends on 1)

The process of claim 1 including,
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide, polyethylene terephthalate and polyvinyl chloride.

### Claim 12 (depends on 1)

The process of claim 1 including,
said filter having a pore size of about 5 microns.

### Claim 13 (depends on 1)

The process of claim 1 including,
removing solid particles and liquid globules of said phosphates and esters with said filtering,
removing hydrolysates of said phosphates and esters with said anion exchange resin, and
removing remaining amounts of said phosphates and esters and said hydrolysates by said sorption.

### Claim 14 (depends on 1)

The process of claim 1 including,
separating said lower and upper layers by decanting, and
said filter for said filtering step having a pore size ranging from 5 to 10 microns.

### Claim 15 (depends on 1)

The process of claim 1 including,
said filter being composed of polypropylene, and
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resin, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines.

### Claim 16 (depends on 1)

The process of claim 1 including,
removing more than 90% of the hydrolysates and substantially none of the phosphates or esters by means of said demineralization,
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride, and
said filter having a pore size of about 5 microns.

### Claim 17 (depends on 1)

The process of claim 1 including,
removing solid particles and liquid globules of said phosphates and esters with said filtering,
removing hydrolysates of said phosphates and esters with said anion exchange resin,
removing remaining amounts of said phosphates and esters and said hydrolysates by said sorption,
removing said lower layer by decanting, and
said filter for said filtering step having a pore size ranging from 5 to 10 microns.

### Claim 18 (depends on 1)

The process of claim 1 including,
said filter being composed of polypropylene,
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines,
removing more than 90% of the hydrolysates and substantially none of the phosphates or esters by means of said demineralization,
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride, and
said filter having a pore size of about 5 microns.

### Claim 19 (depends on 1)

The process of claim 1 including,
removing solid particles and liquid globules of said phosphates and esters with said filtering,
removing hydrolysates of said phosphates and esters with said anion exchange resin,
said removing of hydrolysates with said anion exchange resin being the substantial majority of the hydrolysates present,
removing remaining amounts of said phosphates and esters and said hydrolysates by said sorption,
separating said lower and upper layers by decanting,
said filter for said filtering step having a pore size ranging from 5 to 10 microns,
said filter being composed of polypropylene, and
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines.

### Claim 20 (depends on 1)

The process of claim 1 including,
removing solid particles and liquid globules of said phosphates and esters with said filtering,
removing hydrolysates of said phosphates and esters with said anion exchange resin,
said removing of hydrolysates with said anion exchange resin being the substantial majority of the hydrolysates present,
removing remaining amounts of said phosphates and esters and said hydrolysates by said sorption,
separating said lower and upper layers by decanting,
said filter being composed of polypropylene,
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines,
removing more than 90% of the hydrolysates and substantially none of the phosphates or esters by means of said demineralizaton,
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride, and
said filter having a pore size of about 5 microns.

### Claim 21

The process of removing water from an aqueous mixture of aryl phosphates and esters and hydrolysates thereof comprising,
filtering said mixture with a filter having a pore size of between 1 micron to about 25 microns,
demineralizing the effluent from said filtering with an anion exchange resin,
sorbing remaining said phosphates and esters and hydrolysates from the effluent from said demineralizing with an organic polymeric material sorber, and
collecting substantially clean water from said sorbing step.

### Claim 22 (depends on 21)

The process of claim 21 including,
said filter for said filtering step having a pore size ranging from 5 to 10 microns, and
said filter being composed of polypropylene.

### Claim 23 (depends on 21)

The process of claim 21 including,
said filter for said filtering step having a pore size ranging from 5 to 10 microns,
said filter being composed of polypropylene,
removing more than 90% of the hydrolysates and substantially none of the phosphates or esters by means of said demineralization, and
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride.

### Claim 24

An apparatus for removing water from an aqueous mixture of aryl phosphates and esters and hydrolysates thereof comprising, in the following succession,
decanting means to remove said aqueous mixture from any separate layer of said phosphates and esters and hydrolysates,
filter means having a pore size of between about 1 micron to 25 microns for filtering said mixture,
a demineralizer fluidly connected to said filter means to remove hydrolysates, from said mixture following said filtering,
said demineralizer being an anion exchange resin,
a sorber fluidly connected to said demineralizer, for receiving the effluent from said demineralizer, said sorber being an organic polymeric material for removing remaining amounts of said phosphates and esters and hydrolysates from said mixture to produce substantially clean water.

### Claim 25 (depends on 24)

The apparatus of claim 24 including,
said filter means for said filtering step having a pore size ranging from 5 to 10 microns.

### Claim 26 (depends on 24)

The apparatus of claim 24 including,
said filter means being composed of polypropylene.

### Claim 27 (depends on 24)

The apparatus of claim 24 including,
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines.

### Claim 28 (depends on 24)

The apparatus of claim 24 including,
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride.

### Claim 29 (depends on 24)

The apparatus of claim 24 including,
said filter means for said filtering step having a pore size ranging from 5 to 10 microns, and
said filter means being composed of polypropylene.

### Claim 30 (depends on 24)

The apparatus of claim 24 including,
said filter means for said filtering step having a pore size ranging from 5 to 10 microns,
said filter means being composed of polypropylene,
said anion exchange resin being selected from the group consisting of styrene based quaternary ammonium resins, acrylic based quaternary ammonium resins, styrene-divinylbenzene based amines, acrylic based amines, epoxy based amines, and phenolic based amines, and
said organic polymeric material being selected from the group consisting of polyethylene, polypropylene, polybutylene, polyamide polyethylene terephthalate and polyvinyl chloride.
