-=---
`--~~~~ ~~-=-=-=
`-- ----- - .
`
`--- ---
`
`--=---~- -
`
`·---
`
`POLY OX
`Water-Soluble Resins
`
`Unique Resins for
`Binding, Lubricity,
`Adhesion and Emollient
`Perfonnance
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Table of Contents
`
`3 Introduction
`
`4, 5 A Wide Range of Performance Properties
`
`6-15 Applications
`6,7 Aqueous Drag Reduction and Drift Control
`6,7 Agriculture
`8 Building and Construction
`9 Ceramics
`10 Cleaners, Personal Care and Cosmetics
`12 Electronics and Telecommunications
`13 Mining
`14 Paper
`15 Pharmaceuticals
`
`16-18 Properties ofPOLYOXTM Water-Soluble Resins
`17 Viscosities
`18 Solution Properties, Typical Physical Properties
`
`19 Storage, Compendium Status, EPA Status,
`FDA Status
`
`20-22 Working with POLYOX Water-Soluble Resins to
`Achieve Proper Dissolution
`
`23 Product Safety
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Introduction
`
`POLY OX Water-Soluble Resins are nonionic, high
`molecular weight water-soluble poly (ethylene oxide)
`polymers. Molecular weights range from 100,000 to
`about 8, 000,000. They exhibit many properties
`that are typical of other classes of water-soluble
`polymers -lubricity, binding, water retention,
`thickening, and fllm formation.
`
`But POLYOX Water-Soluble Resins can do even
`more. They're thermoplastic materials that are
`readily calendared, extruded, injection molded, or
`cast. Films of POLYOX Water-Soluble Resins are
`flexible, tough, and resistant to most oils and greases.
`VVith their very high molecular weight, POLYOX
`Water-Soluble Resins are viscoelastic, so their
`aqueous solutions can reduce spattering and misting
`potential. And POLYOX Water-Soluble Resins can
`form association compounds with many other
`substances to achieve a wide variety of additional,
`useful formulation properties .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`High Binding Efficiency
`POLY OX Water-Soluble
`Resins have high-binding
`efficiency for pigments, fillers,
`metal powders and ceramics.
`These binders easily burn off
`at low temperatures with little
`or no tendency to char.
`
`Form Novel Complexes
`The strong hydrogen bonding
`affinity of POLYOX Water-
`Soluble Resins accounts for
`the association of these
`polyethers with various
`polar compounds, such as
`phenolic resins, mineral acids,
`halogens, ureas, lignin
`sulfonic acids and poly
`(carboxylic acids). These
`novel complexes can be
`discrete chemical entities
`resulting from very strong
`intermolecular association
`and often exhibit properties
`markedly different from
`either component.
`
`Crosslinkable
`POLY OX Water-Soluble
`Resins can be crosslinked to
`form gels that are highly
`water-retentive.
`
`Emollient
`When applied to the skin and
`hair, POLY OX Water-Soluble
`Resins produce a soft and
`"silky" feel.
`
`Film Former, Excipient
`POLYOX Water-Soluble
`Resins can be formed into
`flexible films both by
`thermoplastic processing and
`casting techniques. Such films
`may be made of POLY OX
`Water-Soluble Resins alone or
`blended with a wide variety
`of other polymers, such as
`polyethylene, polystyrene,
`polycaprolactone, ethylene
`vinyl acetate, nylon, etc.
`
`Low Toxicity
`POLY OX Water-Soluble
`Resins show a very low order
`of toxicity in animal studies
`by all routes of exposure. At
`the maximum practical oral
`dose to rates of about 2 g/kg
`of body weight there were
`no deaths nor signs of
`toxicity. Because of their high
`molecular weights, the resins
`are poorly absorbed from
`the gastrointestinal tract and
`are completely and rapidly
`eliminated. These resins are
`neither skin irritants nor
`sensitizers, nor do they cause
`eye irritation as the dry
`powder or as aqueous
`solutions.
`
`Flocculant Activity
`High molecular weight grades
`of POLY OX Water-Soluble
`Resins effectively adsorb onto
`many colloidal materials
`and perform as efficient
`flocculating agents. They
`exhibit a high affinity for a
`variety of materials, including
`silica, clays, oxidized coal fines,
`lignins and paper fines.
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Viscoelasticity
`The flexibility of ether linkages
`combined with the extremely
`high molecular weight of
`POLY OX Water-Soluble Resins
`produces solutions with elastic
`behavior. Such solutions will
`climb a rotating shaft! This
`property also tends to reduce
`both the spattering and misting
`potential of aqueous solutions.
`
`Available in Many Grades
`POLY OX Water-Soluble Resins
`are supplied in a wide variety of
`molecular weight grades and
`formulated compounds in
`standard and NF (National
`Formulary) grades.
`
`Wet Tack
`POLY OX Water-Soluble Resins
`exhibit a high degree of wet
`tack and, thus, are useful as wet
`adhesives. The dried residue is
`non-tacky.
`
`Thickening Power
`(Aqueous)
`POLY OX Water-Soluble Resins
`are nonionic and completely
`water-soluble at all tempera-
`tures up to the boiling point of
`water. Unlike most other high
`molecular weight, water-soluble
`resins, they do not exhibit an
`inverse solubility-temperature
`relationship, except near the
`boiling point.
`
`POLYOX Water-Soluble Resins
`are extremely effective thick-
`ening agents in both fresh
`and salt water. Aqueous
`solutions are pseudoplastic
`(i.e., shear thinning).
`
`Drag Reduction!
`Drift Control
`Very low concentrations of the
`higher molecular weight
`POLYOX Water-Soluble Resins
`can reduce the turbulent
`frictional drag of the water in
`which they are dissolved by as
`much as 80 percent.
`
`Lubricity
`POLY OX Water-Soluble
`Resins impart a high degree
`of lubricity when in contact
`with water.
`
`Solubility/Thickening
`of Many Organic Solvents
`POLY OX Water-Soluble Resins
`are readily soluble in and
`will thicken a wide variety of
`organic solvents at various
`temperatures. Typical organic
`solvents include most haloge-
`nated hydrocarbons, various
`ketones, alcohols, aromatic
`hydrocarbons and esters.
`POLY OX Water-Soluble Resins
`are not generally soluble in
`aliphatic hydrocarbon solvents,
`glycols, diols and aliphatic
`ethers.
`
`Thennoplasticity
`As thermoplastics, POL YOX
`Water-Soluble Resins are
`readily calendered, extruded,
`injection molded, or cast.
`Sheets and films of this material
`are heat-sealable and can be
`oriented to develop high
`strength. Films are inherently
`flexible, tough and resistant to
`most oils and greases. These
`resins are compatible with
`many natural and synthetic
`polymers. The combination of
`thermoplasticity and aqueous
`solubility and compatibility
`with "hydrophobic" polymers
`(e.g .. polyethylene,
`polycaprolactone, ethylene
`vinyl acetate, nylon, etc.) make
`POLY OX Water-Soluble Resins
`a valuable asset for degradable
`plastics applications.
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`POLY OX Water-Soluble Resins
`have an unusual array of
`properties that make them
`useful in a wide variety of
`applications. Here's an over-
`view of the many ways they
`can be used and the values
`they bring to so many different
`industries. For more informa-
`tion, see corresponding tables.
`
`Agriculture
`Seed Coatings -As film-
`formers, POLYOX Water-
`Soluble Resins can be used
`in undiluted form as seed
`coatings. POLY OX WSR N-10
`and WSR N-750 products
`are typically used for this
`application.
`
`Aqueous Drag Reduction
`and Drift Control
`Very low concentrations of the
`higher molecular weight
`POLYOX Water-Soluble
`Resins can reduce the turbulent
`frictional drag of the water in
`which they are dissolved by
`as much as 80 percent. Applica-
`tions include agricultural
`sprays, boat hulls, fire-fighting
`additives, fluid jet cutting,
`pipeline slurry transport,
`storm sewers and well-
`fracturing fluids.
`
`Seed Tape- The thermoplastic
`nature and film-forming
`characteristics of POLY OX
`Water-Soluble Resins make
`them ideal for tape coating and
`adhering seed. Because they're
`water-soluble, POLYOX
`Water-Soluble Resins release
`seeds after planting and don't
`interfere with germination and
`growth.
`
`Drift Control- POLY OX
`Water-Soluble Resins are used
`for drift control of agricultural
`sprays, reducing carryover to
`other areas and permitting
`more efficient spray directly
`on foliage.
`
`Water-Soluble Packaging-
`POLY OX Water-Soluble
`Resins can be used as water-
`soluble protective coatings for
`premeasured doses of pesticides
`and other solid agricultural
`formulations .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`----------==-~~
`
`-----~
`
`Recommended grades
`
`Use Levels, PPM
`
`POLYOXWater-5olubi~_Resins in Aqueous Drag Reduction and Drift Control
`\
`~pplication
`Benefi~
`Reduce~1turbulent frictr~nal
`
`Fire-fighting
`additives
`
`WSR-30
`WSR-303
`WSR Coagulant
`
`5-100
`
`drag by \ s much as 80%\
`
`I \ \ \
`\ \
`
`' '
`
`\
`
`Storm sewers WSR-301
`WSR-303
`
`About200
`
`POLYOXWater-5oluble Resins in Agriculture
`
`Application
`
`Seed
`Coatings
`
`Seed Tape
`
`Recommended Use Levels
`grades
`wt%
`WSR N-10
`100
`WSR N-750
`
`WSRN-10
`WSRN-80
`WSR N-750
`
`100
`
`WSR N-10
`WSR-205
`
`Water-
`soluble
`packaging
`Agricultural WSR-301
`drift control
`
`2.0
`
`0.05-0.2
`
`Benefits
`
`Excellent
`film-forming
`characteristics.
`Excellent
`film-forming
`characteristics and
`thermoplasticity.
`Doesn't interfere
`with germination
`and growth of
`seeds after planting.
`Totally water
`soluble; packaging
`dissolves readily.
`Reduced carry over
`to other areas.
`Permits more
`efficient sprays
`directly on foliage .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Building and Construction
`POLY OX Water-Soluble Resins
`are used as thickeners, binders,
`and association compounds
`in paints, coatings, paint
`removers, cements, and
`concrete.
`
`Paints, Coatings, and Paint
`Removers- POLY OX Water-
`Soluble Resins may be used as
`aqueous phase thickeners for
`latex paints. And they're also
`excellent thickeners for many
`organic solvents. POLY OX
`WSR N-750 resin is typically
`used at 3.0 % by weight in
`paint and varnish removers.
`
`Cements and Concrete- In
`cement mortars, POLY OX
`Water-Soluble Resins provide
`aqueous thickening to provide
`proper body and application
`properties. Because they form
`pseudoplastic (shear thinning)
`solutions, they enhance
`workability of cements and
`mortars.
`
`POLYOX WSR-301 resin adds
`excellent lubricity to concrete
`mixes at 0.005 to O.Ql% of
`formulation weight to assist
`pumpability.
`
`POLYOXWater-Soluble Resins in Building and Construction
`Application
`Use Levels Benefits
`Recommended
`grades
`wt%
`
`Paints &
`Coatings
`
`WSRN-750
`
`3.0
`
`Cements&
`Concrete
`
`WSR-301
`
`0.005
`to0.01
`
`Asbestos
`cement
`extrusion
`aid
`Paint and
`varnish
`removers
`Concrete
`pumping
`
`WSR-301
`WSR Coagulant
`
`0.4 based
`on dry
`ingredients
`
`WSRN-750
`
`3.0
`
`WSR-301
`
`0.005-
`0.01
`
`Provides proper
`body and application
`properties. Reduces
`splattering and
`dripping.
`Provides aqueous
`thickening for proper
`body and application
`properties. Also
`forms pseudoplastic
`solutions that enhance
`workability of cements
`and mortars. Film
`forming properties
`provide excellent
`encapsulation of
`mineral powders and
`aggregates.
`Lubricity reduces
`energy requirements
`for extrusion.
`
`Good solubility in
`many organic
`solvents.
`Lubricity assists
`pumping .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Ceramics
`POLY OX Water-Soluble Resins
`are used as binders and forming
`aids in ceramic parts, ceramic
`bricks, ceramic fibers, and
`ceramic extrusion.
`
`In ceramic applications,
`POLY OX Water-Soluble Resins
`serve primarily as binders and
`forming aids. They effectively
`bind components of ceramic
`mixes for the formation of
`
`bricks and ceramic parts. They
`also serve as excellent binders
`for ceramic fibers. For binding,
`POLYOX WSR-301 and
`WSR-303 are typically used at
`0.001 - 0.7% by weight of the
`ceramic mix.
`
`POLY OX Water-Soluble Resins
`also provide excellent lubricity,
`aiding the extrusion of products
`like bricks and asbestos cement.
`
`POLYOXWater-Soluble Resins in Ceramics
`
`Application
`
`Recommended grades
`
`Use Levels, wt%
`
`Benefits
`
`Ceramic
`forming aid
`
`WSR-301
`
`0.001-0.7
`
`Lubricity aids mixing and
`extrusion. High binding
`efficiency. Burns off at low
`temperatures with little
`or no tendency to char .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Cleaners, Personal Care,
`and Cosmetic Products
`POLY OX Water-Soluble Resins
`add many important functional
`and sensory properties to
`cleaners and personal care
`products. Perhaps the most
`valuable is their contribution of
`emollient properties to personal
`care products - hair care
`products, creams, and lotions
`get the smooth, soft feel that
`consumers expect. POLYOX
`Water-Soluble Resins also
`serve as thickeners, binders,
`lubricants, and water-retention
`agents in many other cleaning
`and personal care products.
`
`Cleaners- POLY OX Water-
`Soluble Resins can be used to
`thicken both aqueous cleaners
`and those containing many
`organic solvents. They also act
`as emollients in liquid deter-
`gents like dishwashing liquids.
`With their film-forming activity,
`POLY OX Water-Soluble Resins
`can be used for water-soluble
`packaging of solid detergent
`products. POLYOX Water-
`Soluble Resins add lubricity to
`polishes and waxes for easier
`application.
`
`Hair Care Products- In
`shampoos and conditioners,
`POLY OX Water-Soluble Resins
`serve as emollients and aqueous
`thickeners. They also add
`aqueous thickening to hair set
`lotions.
`
`Skin Care Products- POLY OX
`Water-Soluble Resins are
`outstanding emollients for
`creams and lotions, providing
`a soft feel and smooth applica-
`tion. These resins are also
`crosslinkable to form water-
`retentive matrices for cosmetic
`gels.
`
`Shaving Products- POLY OX
`Water-Soluble Resins provide
`the primary lubricant action in
`lubricant strips for razors -
`injection molded, or cast to the
`desired shape. In shaving gels,
`POLYOX Water-Soluble Resins
`work as emollients and
`lubricants.
`
`Oral Care Products- POLY OX
`Water-Soluble Resins provide
`excellent thickening with low
`toxicity in toothpaste, mouth-
`washes, and denture creams.
`They also provide wet tack for
`dental cements and dental
`adhesives .
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`POLYOXWater-5oluble Resins in Cleaners, Personal Care and Cosmetic Products
`
`Application
`
`Recommended grades
`
`Use Levels, wt%
`
`Benefits
`
`Creams
`and lotions
`
`WSR-205
`WSRN-60K
`
`0.25-0.75
`
`Cold Cream
`
`WSR-205
`
`Denture
`adhesives
`
`Denture
`creams
`Detergent
`liquids
`
`WSR-301
`
`WSR-301 NF
`
`WSRN-3000
`
`0.5
`
`0.5
`
`12-15
`
`0.05-0.1
`
`Hair
`conditioner
`
`WSR-205
`
`0.25
`
`Provides a soft feel and
`smooth application. The
`resins are also crosslinkable
`to form water-retentive
`matrices for cosmetic gels.
`Provides a soft feel and
`smooth application. The
`resins are also cross linkable
`to form water-retentive
`matrices for cosmetic gels.
`Provides excellent thickening
`with low toxicity, plus
`wet tack.
`Provides excellent thickening
`with low toxicity.
`Thickens aqueous cleaners,
`acts as an emollient. Film-
`forming activity useful for
`water-soluble packaging of
`solid detergent products.
`Provides a soft feel and
`smooth application, also
`adds aqueous thickening.
`Provides a soft feel and
`smooth application. Excellent
`binding properties.
`
`Provides a soft feel and
`reduces astringent sensation.
`Provides a soft feel and
`smooth application, also
`adds aqueous thickening.
`Provides a soft feel and
`smooth application; lubricant
`action reduces razor drag.
`Provides the primary
`lubricant action in lubricant
`strips for razors.
`
`Provides excellent thickening
`with low toxicity .
`
`•
`
`Hand soaps
`WSRN-750
`{bar and liquid) WSRN-3000
`WSR-205
`WSR N-12K
`WSRN-60
`WSR-301
`
`Rubbing
`alcohol
`Shampoos
`
`Shaving gels
`
`WSRN-750
`WSR-205
`WSRN-60K
`WSR-205
`
`Shaving/Razors WSRN-80
`WSR N-750
`WSR-301
`WSR Coagulant
`WSR-205 NF
`
`Toothpaste
`
`0.1-1.5
`
`0.1-2.0
`0.2
`0.3
`0.1
`
`0.25-0.5
`
`0.1
`
`50-75
`
`0.3-1.0
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Electronics and
`Telecommunication
`Batteries- POLY OX Water-
`Soluble Resins are used as
`binders for battery electrodes
`and separators for batteries.
`They can dissolve a large
`amount of the inorganic salts
`and therefore can be used as
`ionically conductive polymer
`electrolytes in rechargeable
`batteries. The polymer electro-
`lytes can be made into strong
`and flexible thin films to
`improve the battery safety and
`performance. This approach
`also opens the door to new
`battery designs.
`
`Fluorescent Lamps and
`Cathode Ray Tubes- POLY OX
`Water-Soluble Resins are widely
`used as binders for fluorescent
`lamp phosphors. POLYOX
`WSRN-750 and N-3000 are
`typically used at concentrations
`of 1-5%. These polymers also
`see utility as phosphor binders
`in cathode ray tubes.
`
`Wire, Cable, and Optical
`Fibers- To assist in assembly
`and installation operations,
`POLYOX Water-Soluble Resins
`may be used as lubricants for
`wire, cable, and optical fibers.
`
`POLYOXWater..Soluble Resins in
`Electronics and Telecommunications
`Application Recommended Use Levels Benefits
`grades
`wt%
`WSRN-750
`20-80
`WSRN-80
`
`Batteries
`
`Efficient binding for
`battery electrodes.
`Form ionically
`conducting polymer
`electrolytes with
`many inorganic salts.
`
`Wire, Cable WSR-301
`and Optical
`Fibers
`Fluorescent WSRN-750
`WSRN-3000
`lamp
`phosphor
`binder
`
`0.1
`
`0.1-2.0
`4.0-6.0
`
`Lubricity aids in
`assembly and
`installation operations.
`Burn off at low
`temperatures
`with little or no
`tendency to char.
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Mining
`POLY OX Water-Soluble
`Resins are used extensively as
`flocculating agents in mining
`operations. High molecular
`weight grades ofPOLYOX
`Water-Soluble Resins, sold
`under the UCARFLOC™
`name, effectively adsorb onto
`many colloidal materials and
`perform as efficient flocculating
`agents. They exhibit a high
`affinity for a variety of materials,
`including silica, clays, and
`oxidized coal fines. See the
`table at right.
`
`POLY OX Water-Soluble Resins
`are used as lubricants and drag
`reduction agents for pipeline
`slurry transport. They also have
`utility as dust suppressants.
`
`
`
`oc u UCARFLOC Fl c lating Agents In Mining Applications
`
`Benefits
`
`High affinity for many materials;
`effective adsorption onto
`surfaces and efficient
`flocculating action.
`
`Use Levels
`5 ppm-0.2%
`of total clay
`suspension
`
`O.D1-0.1%
`of solids
`
`O.D1 to 0.1%
`of slurry solids
`
`O.D1- 0.1%
`of clay solids
`
`10 -20 ppm
`
`5-10 ppm
`
`2.0
`
`Excellent film formation.
`
`Recommended grades
`Application
`Clay suspensions UCARFLOC 302
`UCARFLOC 304
`UCARFLOC 309
`
`Heavy metal
`ore flocculation
`
`Oxidized
`coal slurries
`
`Phosphate
`slimes
`
`Rock drilling
`enhancer
`
`Silica
`suspensions
`
`Reducing
`spontaneous
`combustion
`of coal
`
`UCARFLOC 300
`UCARFLOC 302
`UCARFLOC 309
`
`UCARFLOC 302
`UCARFLOC 304
`UCARFLOC 309
`
`UCARFLOC 300
`UCARFLOC 304
`
`UCARFLOC 300
`
`UCARFLOC 302
`UCARFLOC 304
`UCARFLOC 309
`
`WSRN-750
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Paper
`In papermaking, POLY OX
`Water-Soluble Resins serve as
`processing aids and compo-
`nents of fmished products.
`Their primary roles are as
`adhesives and flocculants.
`
`Adhesives- Solutions of
`POLY OX Water-Soluble Resins
`exhibit a high degree of wet
`tack and thus are useful as
`wet adhesives for tail-tie
`applications, and in tissue and
`toweling. The dry residue is
`non-tacky
`
`Flocculation- High molecular
`weight grades of POLY OX
`Water-Soluble Resins, sold
`under the UCARFLOC name,
`are used in paper making due
`to their high affinity for pulps,
`fillers, and pitch. POLY OX
`Water-Soluble Resins are used
`in fmes retention, drainage
`enhancement and in paper
`waste systems. They exhibit a
`high affinity for a variety of
`materials, including silica, clays,
`lignins, and paper fines.
`
`UCARFLOC Flocculating Agents In Paper Applications
`
`Application
`Tail-tie paper
`adhesives
`
`Tissue and
`toweling
`adhesives
`
`Flocculation and
`
`Recommended grades
`POLYOX WSR N-750
`POLY OX WSR-205
`POLYOX WSR-301
`
`POLYOX WSR N-750
`POLYOX WSR-205
`POLYOX WSR N-3000
`
`UCARFLOC 300
`UCARFLOC 302
`UCARFLOC 304
`UCARFLOC 309
`
`Use Levels wt%
`3-7
`
`4-7
`
`0.005-0.25
`of dry fiber
`
`Benefits
`High degree of wet-tack
`with dry residue that's
`non-tacky.
`
`High degree of wet-tack
`with dry residue that's
`non-tacky.
`
`High affinity for a variety
`of materials; efficient
`flocculation.
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Phannaceuticals
`POLYOX Water-Soluble Resins
`NF are nonionic poly( ethylene
`oxide) polymers. They meet
`the requirements of the Food
`Chemicals Codex, the Interna-
`tional Codex Alirnentarius and
`US Pharmacopoeia (USP) or
`National Formulary (NF).
`These products have also been
`approved in drug products sold
`in Britain and m~or European
`countries. They are white, free-
`flowing hydrophilic powders
`supplied in a wide variety of
`molecular weight grades,
`ranging from one hundred
`thousand to eight million.
`POLY OX Water-Soluble Resins
`NF have a long history of
`successful applications in
`pharmaceutical products, in
`uses such as controlled release
`solid dose matrix systems,
`tablet binding, transdermal
`drug delivery systems, and
`mucosal bioadhesives.
`
`Controlled Release Matrix
`Systems- POLY OX Water-
`Soluble Resins NF are very
`versatile polymers for con-
`trolled release applications.
`Upon exposure to water or
`gastric juices, they hydrate and
`swell rapidly to form hydrogels
`with properties ideally suited
`for controlled drug-delivery
`vehicles. Because POLY OX
`Water-Soluble Resins NF are
`nonionic, no interaction
`between drug and polymers is
`to be expected.
`
`form a strong interpenetrating
`network with mucus. Data
`indicate that molecular weights
`of 4,000,000 and higher have
`the highest level of adhesion.
`
`Melt Extrusion- POLY OX
`Water-Soluble Resins NF
`provide good flow characteris-
`tics and can be used in conven-
`tional equipment.
`
`Direct Compression Tablet
`Binding- POLY OX Water-
`Soluble Resins NF perform well
`as binders in direct compression
`systems. They often provide
`better flow and compaction
`properties than other binders.
`And their lubricity also assists
`tableting operations.
`
`Mucosal Bioadhesives-
`POLYOX Water-Soluble
`Resins NF offer a number of
`important properties for
`mucoadhesion -water solubil-
`ity, hydrophilicity, high
`molecular weight, hydrogen
`bonding functionality, and
`good biocompatibility. These
`resins have a long linear chain
`structure which allows them to
`
`POLYOXWater-5oluble Resins NF for Phannaceutical Applications
`POLYOX
`Approximate
`Viscosity Range at 25°C, cP
`Water-soluble
`Molecular
`Resin NF Product
`Weight
`
`5% Solution
`
`2%Solution
`
`1% Solution
`
`30-50
`55-90
`600-1,200
`4,500-8,800
`8,800-17,600
`
`WSRN-10
`WSRN-80
`WSRN-750
`WSR-205
`WSR-1105
`
`WSR N-12K
`WSRN-60K
`
`WSR-301
`WSR Coagulant
`WSR-303
`
`100,000
`200,000
`300,000
`600,000
`900,000
`
`1,000,000
`2,000,000
`
`4,000,000
`5,000,000
`7,000,000
`
`400-800
`2,000-4,000
`
`1,650-5,500
`5,500-7,500
`7,500-1 0,000
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Table1
`
`Grades of POLYOXWater..Soluble Resins
`Approximate Molecular Weight (ll
`POLYOX Grade
`
`WSR N-10
`WSRN-80
`WSRN-750
`
`WSRN-3000
`WSR-205
`
`WSR-1105
`WSR N-12K
`WSRN-60K
`
`WSR-301
`WSR Coagulant
`WSR-303
`WSR-308
`UCARFLOC Polymer 300
`UCARFLOC Polymer 302
`UCARFLOC Polymer 304
`UCARFLOC Polymer 309
`
`POL YOX NF Grades
`
`100,000
`200,000
`300,000
`
`400,000
`600,000
`
`900,000
`1,000,000
`2,000,000
`
`4,000,000
`5,000,000
`7,000,000
`8,000,000
`4,000,000
`5,000,000
`7,000,000
`8,000,000
`
`The physical property data listed are considered to be typical properties,
`not specifications.
`
`(1) Based on rheological measurements. Molecular weights obtained by other
`methods, including light scattering and gel permeation chromatography, may
`not be directly comparable.
`(2) Model RVT.
`(3) POLY OX Water-Soluble Resins NF comply with The National Formulary
`standard for "Polyethylene Oxide" (page 2285-6) in USP 23-NF 18
`issued in 1995 .
`
`POLYOX Water-Soluble Resins
`are supplied in a wide variety
`of molecular weight grades
`and formulated compounds in
`standard and NF (National
`Formulary) grades. Table 1
`shows the current product
`range and their corresponding
`molecular weights and proper-
`ties. Figure 1 summarizes the
`solution properties of each
`type. Both thickening efficiency
`and pituity (i.e., viscoelastic
`behavior) increase with
`increasing molecular weight.
`
`POLY OX Water-Soluble Resins
`are produced and supplied as
`white, granular powders, freely
`soluble in water and possessing
`a slightly ammoniacal odor.
`Typical properties are given in
`Table 2.
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Viscosity Range, mPa • sec (cP), Aqueous Solution at 25°C, Weight Percent
`
`Brookfield Viscometer, Model RVF,
`Spindle No./Speed, rpm
`
`5%
`
`12-50
`65-115
`600-1000
`1000-1200
`
`2250-4500
`4500-8800
`
`8800-17,600
`
`2%
`
`1%
`
`400-800
`2000-4000
`
`1650-5500
`5500-7500
`7500-10,000
`10,000-15,000
`1650-5500
`5500-7500
`7500-10,000
`10,000-15,000
`
`Contact your Dow representative regarding resins that meet the NF standard (Jl •
`
`1/50 (2)
`1150 (2)
`1/10
`2/10
`
`1/2
`2/2
`
`2/2
`1/10
`3/10
`
`2/2
`2/2
`2/2
`2/2
`2/2
`2/2
`2/2
`2/2
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Figure1
`
`Molecular
`Weight
`:2:4,000,000
`
`Solution Properties of POLYOXWater-5oluble Resins
`Viscoelasticity
`Shear Thinning
`(Pituity)1
`(Pseudoplasticity)
`...
`~~
`\':.•:-,.
`·· ....
`·····~
`
`€ 8
`
`~
`
`j '
`t ~ "-------
`
`Mechanical Shear
`Durability
`
`1J
`<ll
`.!:;
`!!l
`<ll a::
`% 8
`
`~
`
`1J
`<ll
`.!:;
`!!l
`
`<ll a:: t ~
`
`Shear Exposure
`
`Shear Exposure
`
`Shear Rate
`
`Shear Rate
`
`'·· ,.._
`
`Molecular
`Weight
`<4,000,000
`
`~,.,
`
`·,~,-~
`
`;:. .:.
`.:.
`
`Table2
`
`1 Increases with molecular weight
`
`Appearance
`Crystalline Melting Point <1l (X-ray and DSC), ac
`Odor
`Melt Flow Temperature, ac
`Volatiles Content, as
`Alkaline Earth Metals, % by wt as CaO, max
`Powder Bulk
`Ib/ftJ
`Polymer Density, glee
`Moisture Content, as
`Heat of Fusion, cal/gm
`Solution
`Particle Size, % by wt
`Average through 1 0-mesh (U.S. Standard)
`20-mesh
`
`%
`
`Off-white powder
`62-67
`Sl
`
`ammoniacal
`
`> 98
`> 1.0
`1.0
`19-37 (304-593)
`1.15-1.26
`<1
`33
`8-10
`
`100
`96
`
`The physical property data listed are considered to be typical
`properties, not specilications.
`
`W At temperatures far above the crystalline melting point, high
`polymers of POLY OX Water-Soluble Resins still retain a ve.ry
`high degree of crystalline character.
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Storage Stability
`POLYOX Water-Soluble Resins
`will degrade to lower molecular
`weights with time and elevated
`temperature. Higher molecular
`weight grades are more
`sensitive than lower molecular
`weight grades. Samples past
`their expiration date should be
`evaluated to confirm that they
`are within specification limits.
`Samples that are out of
`specification should be
`discarded.
`
`Compendium Status
`NF (National Formulary)
`grades ofPOLYOXWater-
`Soluble Resins are available.
`POLY OX Water-Soluble Resins
`NF are identified in the
`Compendium as Polyethylene
`Oxide.
`
`EPA Status
`POLY OX Water-Soluble Resins
`are identified by the Federal
`Environmental Protection
`Agency in 40 CFR 180.1001
`(d) for unrestricted use as inert
`ingredients in pesticide formu-
`lations applied to crops up to
`the time of harvest.
`
`FDA Status
`Considerable interest has been
`shown in POLYOX Water-
`Soluble Resins for diverse
`applications in food, drug and
`cosmetic products. Such uses
`fall within the scope of the
`Federal Food, Drug and
`
`Cosmetic Act. The FDA has
`recognized and approved the
`use of Poly( ethylene oxide)
`polymers (POLYOX Water-
`Soluble Resins) for specific food
`packaging uses, and as a direct
`additive to beer.
`
`Table3
`
`FDA Status of POLYOX Water-Soluble Resins
`FDA Regulation
`(21 CFR)
`172.770
`
`Permitted Uses
`Foam stabilizer in fermented malt
`beverages (not to exceed 300 ppm by
`weight of the beverage) (WSR-301 and
`higher molecular weight grades).
`Component of resinous and polymeric
`coatings applied as a continuous film or
`enamel over a metal substrate or
`applied as a continuous film or enamel
`to any suitable substrate provided that
`the coating serves as a functional barrier
`between the food and the substrate and
`is intended for repeated food-contact use
`(all grades).
`Aqjuvant in the production of or added
`to impart desired physical and technical
`properties to xylene-formaldehyde
`resins condensed with 4,4'-isopropylidene-
`diphenol-epichlorohydrin epoxy resins
`for use in coatings in contact with
`aqueous and dry foods, and beverages
`(all grades).
`Preparation of zinc-silicon dioxide matrix
`coatings used as food-contact surfaces
`for bulk reusable containers intended for
`storing, handling and transporting food
`(all grades).
`Component of the coated or uncoated
`food-contact surface of paper and
`paperboard in contact with fatty,
`aqueous, and dry food (all grades).
`Manufacture of closures with sealing
`gaskets for food containers (all grades).
`Adjuvant in the manufacture of
`ethylene-vinyl acetate copolymers used
`in food-contact applications (all grades) .
`
`175.300 (xxxiii)
`175.300 (b) (3) (xxxiii)
`
`175.380
`
`175.390
`
`176.170
`176.180
`
`177.1210
`
`177.1350
`
`•
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`Although POLY OX Water-
`Soluble Resins are totally
`water-soluble, care must be
`taken to make sure that they
`are dissolved completely.
`Detailed procedures and
`equipment recommendations
`for laboratory and commercial
`scale methods for dissolving
`POLY OX Water-Soluble
`Resins are described in this
`book.
`
`Which technique you use will
`depend on the fmal viscosity
`and volume required.
`
`For laboratory and less than
`drum quantities, direct addition
`of the POLYOX Water-Soluble
`Resins to water, or non-solvent
`predispersion of POLY OX
`Water-Soluble Resins is
`recommended. For large
`volumes or continuous
`operation, special mechanical
`devices are available. Each
`of these techniques is
`described here.
`
`Direct Addition to Water
`The relative ease of dissolving
`POLY OX Water-Soluble Resins
`directly in water depends on
`three factors: (a) rate of
`viscosity buildup (which is a
`function of solution concentra-
`tion and molecular weight), (b)
`particle size, and (c) type of
`agitation employed. The
`underlying factor, once again, is
`to obtain good resin dispersion
`before the solution viscosity
`builds to a point where it is no
`longer possible to disperse
`additional resin without high
`shear. This is best accomplished
`by adding the POLY OX
`Water-Soluble Resins at just the
`"right" rate of addition. Ifyou
`add it too slowly, the viscosity
`will build too rapidly; and you
`will not be able to add the rest
`of the resin. On the other hand,
`if you add the resin too rapidly,
`it will clump up and not
`dissolve.
`
`The key to dissolution is good
`initial dispersion.
`The most important step in the
`entire dissolving operation of
`POLY OX Water-Soluble
`Resins takes place in the first
`few seconds-separating the
`individual resin particles from
`each other.
`
`High-shear agitators are not
`necessary and should be
`avoided.
`In water, POLYOX Water-
`Soluble Resins are instantly
`wettable. If the POLYOX
`Water-Soluble Resin powder is
`not properly dispersed, the
`partially dissolved, wetted
`particles will agglomerate and
`form gels that may never
`dissolve. High-speed agitation
`of dissolved POLY OX Water-
`Soluble Resins must be avoided
`to prevent shear degradation of
`the resin. Organic solvents,
`because of their lower polarity,
`do not solvate ("wet")
`POLY OX Water-Soluble Resins
`as rapidly as water. As a result,
`particle agglomeration and gel
`formation are generally not
`problems when dissolving
`POLY OX Water-Soluble Resins
`in organic solvents.
`
`Three major techniques
`provide good dispersion of
`resin particles.
`For laboratory or plant
`requirements, these techniques
`fall into three major categories:
`• Simple direct addition to
`water.
`• Predispersion in water-
`miscible non-solvents.
`• Use of mechanical devices
`that achieve dispersion with
`minimal shear.
`
`•
`
`\
`
`KASHIV1045
`IPR of Patent No. 9,492,393
`
`

`

`After about one minute, the
`stirring rate should be reduced
`to about 50-60 rpm. The
`source of heat is then removed
`and a stirring rate of 50-60 rpm
`is continued until solution is
`complete. This technique is
`adaptable to small-and
`medium-size dissolving
`operations, where minimal
`agitation equipment is
`available.
`
`Figure3
`Multi-propeller-type Stirrer
`
`Shaft-
`
`Hot Water Method
`POLY OX Water-Soluble Resins
`are completely soluble in water
`at all temperatures, except near
`the boiling point. At this
`temperature, POLYOX Water-
`Soluble Resins prec