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K-FLEX SHOWCASE

King Industries, Inc. Products for Colorants and Tint Bases

November 2012


High Solids and Waterborne Resins for Colorants


K-FLEX Products for Higher Solids SB and WB Pigment Grinds • Higher solids SB pigment grinds with K-FLEX Polyesters • Higher solids WB pigment grinds with K-FLEX Urethane diols


K-FLEX Polyester Benefits (Features) • • • • • • • • • •

Light stable (aliphatic and saturated) Low VOC (low MW, narrow MWD) Good flexibility (polyester backbone) Fast cure, lower temperature cure (primary hydroxyls only) Water/humidity resistance (sterically hindered esters and overall composition) Hydrolysis resistance (no acid functionality) Excellent compatibility with many resins (narrow MWD) Great solubility in many solvents including exempt solvents for the US and Canada (narrow MWD) Efficient viscosity reduction (narrow MWD) Minimal gassing with NCO (typical water is 0.02%)


K-FLEX Benefits (Features) • • • • • • •

Excellent adhesion to many substrates including plastics (low MW and primary hydroxyl groups) Excellent abrasion (mar) resistance (hardness with flexibility) Non-toxic (low concern polyols) Solvent-free (all in this presentation are supplied 100%) Range of properties (varying Tg and composition) Regulatory compliance globally Possible to formulate higher solids pigment grinds


K-FLEX Polyester Polyol Range Comparison K-FLEX

Appearance

Viscosity cPs, 25째C

OH #

APHA

Refractive Index

Tg 째C*

XM-337

Clear Liquid

70,000

220

20

1.4974

-20

188

Clear Liquid

10,520

231

20

1.4927

-32

A307

Clear Liquid

5,400

140

20

1.4832

-50

XM-366

Clear Liquid

2,000

265

20

1.4787

-45

A308

Clear Liquid

1,500

252

20

1.4810

-59

XM-332

Clear Liquid

450

260

20

1.4672

-68


Polyol Modifier Viscosity vs VOC 80000 70,000

400

407 350

60000 343

339

336

337

334

300

50000 250 40000

All system VOC’s are for 600 cPs Formulation viscosity at 25°C 14% K-FLEX on TRS

30000

200 150

20000

100 10,000

10000

50 2,000

1,500

400

XM-366

A308

XM-332

0

0 Acrylic Control

XM-337

188

K-FLEX Modifier of Joncryl 906 Polyol Viscosity

VOC (g/l)

VOC Formulation (g/l)

K-FLEX Modifier Viscosity, cPs at 25°C

70000

450


Modifier in Pigmented Acrylic 2K PU Joncryl 906/Polyol/Desmodur N-3300 2 Week Ambient Cure Properties 14% TRS K-FLEX

Pendulum Pencil Hardness Hardness

Reverse Impact Res. (in-lbs)

Direct Impact Res. (in-lbs)

J-906

121

2-3H

20-30

90-100

XM-337*

118

3-4H

120-130

160+

188**

116

2-3H

160+

160+

XM-366***

106

2-3H

160+

160+

A308

110

2-3H

160+

160+

XM-332

77

H-2H

160+

160+

*XM-337 Formulation API-16 **188 Formulation API-17 ***XM-366 Formulation API-15

All films had 100% crosshatch adhesion and 100 MEK 2X rubs


Reverse Impact Acrylic Control

Failure 160 in-lbs

Acrylic Control

Failure 160 in-lbs Magnified

Acrylic Control

K-FLEX XM-366

Failure 5 in-lbs Magnified

Pass 160+ in-lbs


92% High Solids Pigment Dispersion Grind Grind (Ball Mill) Description

Weight

K-FLEX 188

Polyester Polyol

12.0

Acrylic

Pigment Wetter

2.5

Methanol

Solvent

3.7

K-SPERSE 152

Monomeric Dispersant

0.3

Ti-Pure R-960

TiO2 Pigment

33.7

Total

52.2

Formulation PM-8 – Pigmented Polyol/Melamine Adhesion To Plastic Substrates


High Solids Pigment Dispersion Grind Grind (Ball Mill) Description

Weight

Grind

Pigment Dispersion

52.2

K-FLEX 188

Polyester Polyol

14.8

Methanol

Solvent

10.0

N-Butanol

Solvent

1.5

HMMM

Crosslinker

19.1

K-CURE 129B

Catalyst

2.4

Total

100.0

Formulation PM-8 – Pigmented Polyol/Melamine Adhesion To Plastic Substrates


Formulation Parameters K-FLEX 188: HMMM

58:42

Pigment: Binder

0.7:1.0

VOC (60’/110°C)

288 g/l (2.40 lbs/gal)

% Resin Solids

48%

% Total Solids

92%


K-FLEX Urethane Diol Structure O O II II HO \/\/\ OCNH \/\/\/\ NHCO /\/\/ OH


Features (Benefits) K-FLEX Urethane Diol •

Aliphatic Saturated Urethane – Light Stability – Hardness – Chemical Resistance

Low MW, Narrow MWD – – – – –

• •

Low Viscosity Low VOC Water soluble without co-solvent, amine or surfactant Co-solvent replacement (partial or total) Improved Flow and Leveling

Hydroxyl Functional (Crosslinks melamine or NCO) No Acid Functionality (won’t catalyze hydrolysis)


Typical Properties K-FLEX Urethane Diol Properties Form*

UD-350W Water Solution

% Active

88

Solvent

Water

Viscosity, Poise

30

OH # (As Supplied)

325

Water soluble without amine, without co-solvent and without surfactant


K-FLEX UD-320-100 Co-Solvent Viscosity Reduction for WB Systems Initial Viscosity 157,0000, 25째C, cPs

Viscosity, 25째C, cPs

100000 10000 1000 100 10 88

84

80

76

72

68

64

60

% Non-Volatile 2-ButoxyWater

ethanol

2-Methoxy-propanol Methanol

i-Propanol


VOC Reduction K-FLEX UD-350W in Waterborne Formulations (60min/110oC) Modification Level

% Decrease in VOC (Calc.)

Joncryl 540/HMMM

5.0%

65.6

Kelsol 3961-B2G-75/HMMM

10%

11.0

Acrysol WS-68/HMMM

13%

8.0

Main Binders


Initial Gloss (20o and 60o)

Gloss 20째/60째

Joncryl 540 Emulsion/HMMM Modification 95 85 75 65 55 45 0

5

10

% K-FLEX UD-320W 60o Gloss 20o Gloss

15


QUV 60 Gloss (1,200 hrs) o

Joncryl 540 Acrylic Emulsion/HMMM 45 40 60째Gloss

35 30 25 20 15 10 0

5

10

% K-FLEX UD-320W on TRS 1200 Hours

15


K-FLEX UD-350W AntiSkinning Versus Dowanol DB

DOWANOL DB

UD-350W

Joncryl 540 acrylic emulsion with 11% Dowanol DB versus 11% K-FLEX UD-350W overnight skinning


Resistance Properties Urethane Diol Modification Main binder

Polymac 72-7203 Water Reducible Polyester

Kelsol 301-W-39 Polyester Dispersion

15% K-FLEX Modification

Boiling Salt Spray Humidity Water Resistance Resistance Resistance

Control

8D

4D/2

5

UD-350W

10

4F/1

59

Control

6D

4D/10

79

UD-350W

10

4D/3

82

Blisters: 1 = Big, 10 = No attack, F = Few, D = Dense


Stain Resistance Duramac 74-7412/HMMM (% K-FLEX UD-320W Modification)

Household Item Isopropanol Mustard Bleach Liquid Cleaner Nail Polish Remover Coffee Homogenized Milk Ketchup Pepsi Cola Mineral Oil Water Lemon Juice

0%

5%

10%

Severe Attack Mild Attack No Effect Severe Attack Severe Attack Severe Stain Severe Attack Superficial Stain Mild Attack No Effect Stain Mild Attack

Severe Attack Mild Attack No Effect Severe Attack No Effect Severe Stain No Effect No Effect Mild Attack No Effect Stain Severe Attack

Severe Attack No Effect No Effect Severe Attack No Effect Mild Stain No Effect No Effect No Effect No Effect Stain Severe Attack


3 Years FL Exposure (5o South) 20 Gloss, % Reflectance

Desmophen 651A-65/K-FLEX UD-320-100/Tolonate HDB-75BX 90 85 80 75 70 0

3

6

9

12

15

18

21

27

Months in FL Polyester Control

• • • • •

K-FLEX UD-320-100

Formulation PI-9 update CC over white BC 5% UD-320-100 on TRS UD-320-100 higher hardness & flexibility UD-320-100 improved gloss retention in QUV

30

36


K-FLEX XM-3307 Typical Properties/Solubility

• • • • • •

Typical Properties Polyester-urethane OH # 35 AV 56 80% Solids in xylene Viscous liquid Molecular Weight 1,500 g/mole

• •

Solubility Soluble in: alcohols, esters, ketones, aromatic hydrocarbons Soluble in water with a neutralizing amine Insoluble in aliphatic hydrocarbons


K-FLEX XM-3307 Applications • Dispersing resin for organic and inorganic pigments • Short dispersion time • High transparency of pigments • High pigment loading • For water (with neutralizing amine) and solvent based systems


DISPERSANTS


K-SPERSE Wetting and Dispersing Additives •

•

Dispersants for solventborne and solvent free formulations Effective for dispersing organic and inorganic pigments


KSPERSE DISPERSANT TYPES For SB Systems

• Polymeric – For use with organic and carbon black – Does not require a wetting resin – Higher cost

• Monomeric – For use with inorganic and carbon black – Require a wetting resin – Lower cost


K-SPERSE Monomeric Interaction Hydrophobic Tail

Polar Sulfonate

-

K-Sperse wets out the pigment and passivates the pigment surface, preventing reflocculation by eliminating the attraction of their charged surfaces.

+-

+ + + +

PIGMENT

+ + +

+ -


Monomeric Product Information • Ca and Zn salts of Alkyl Naphthalene Sulfonic Acid • Products vary in diluent


Monomeric Dispersant Products • K-Sperse 131 - Ca Salt in Mineral Spirits • K-Sperse 152MS - Zn Salt in Mineral Spirits • K-Sperse 152 - Zn Salt in Butoxyethanol


Monomeric Dispersants: Applications • 152 and 152MS (Zinc Salts) for most resin systems and applications • 131(Calcium Salt) for systems containing epoxies, urethanes or where zinc could react • 132/PAO and 152/PAO for 100% solids inks, gel coats


Pigment Successes • • • • • •

Carbon Black - Cabot, Degussa Phthalocyanine Blue - Red Shade Iron Oxides: Red,Yellow,Black Rutile TiO2 Napthol Red - Yellow Shade Mostly with K-Sperse 152/152MS


K-SPERSE Monomeric Use Levels - Except Carbon Black lbs K-Sperse/100 lbs Pigment

% of K-Sperse on pigment weight is 0.05 g/m2 x Pigment Surface Area

5 4.5

4 3.5

3 2.5

2 1.5

1 0.5

0

0

20 *Iron *TiO 2 Extenders Oxides

40 *Organic

Pigments

60 *Phthalo

Blue

Pigment Surface Area m2/g

80 *Transp. 100

Iron Oxide


K-SPERSE Monomeric Use Levels - Carbon Black lbs K-Sperse/100 lbs Pigment

% of K-Sperse on pigment weight is 0.013 g/m2 x Pigment Surface Area 14

12

10

8

6

4

2

0 0

100

200

300

400

*Regular Color *Medium

500

600

700

800

High

*

Pigment Surface Area m2/g

900

1000


Weight % Dispersant on Pigment K-SPERSE

Competition

3.5%

10-33%

7-35% 7%

100% 17-100%

Trans. Fe Oxide

5%

7-30%

Chromopthal Red

8%

12-15%

1.5%

2.5%

0.2-0.6%

1.2%

Phthalo Blue - Red Shade

Carbon Black -Furnace Black -Channel Black

Iron Oxide Titanium Dioxide


Evaluation with Carbon Black Competitive Evaluation – Solsperse 2400/5000, Byk 163, Efka 46, Ser-Ad FA196 – AT-400 Acrylic/Melamine Bake Enamel – Monarch 1300 High Color Carbon Black – Steel Shot Mill – Solvent - MEK


K-SPERSE Monomeric Advantages • Milling time reduction • Higher gloss due to better dispersing • Higher pigment loading (efficiency): 50-75% lower dispersant demand • Lower viscosity carbon black dispersions • Better color development • USE with good WETTING RESIN!


0 Ser-ad FA 196

Efka 46

Byk 163

KSPERSE 152

Solsperse

Higher Gloss

100

80

60

40 Gloss 60째

20 Gloss 20째


Lower Viscosity 80000 1.5rpm 0.6rpm 0,3rpm

60000 40000 20000

FA 196

Ser-ad

Efka 46

Byk 163

KSPERSE 152

Solsperse

0


Graph of Viscosity versus Dispersant demand Dispersant Demand Chart 180000 160000 Viscosity (cps)

140000 120000

K-SPERSE 152

100000

ANTI-TERRA U

80000 60000 40000 20000 0 0.05

0.15

0.4

0.8

1.2

1.6

% Dispersant on Pigment (TiO2)

King formulation KSP-1

2


Dispersant Effect on Rheology for K-SPERSE速 152 Dispersant Effect on Rheology - K-SPERSE 152

Viscosity (cps)

1600 1400

0.0%

Strongly Dilatant

1200

1.5%

1000

2.0%

Slightly Dilatant

800 600

3.0% New tonian

400 Slightly Thixotropic

200 0 6

12

30

Shear Rate (Brookfield RPM) King formulation KSP-2

60


DISPARLON Paste Thixotropes

NEW DISPARLON BB102

• • • •

Polyamide paste thixotropes for solventborne coatings Cost effective Excellent anti-settling and anti-sag performance Variety of solvent carriers


DISPARLON BB-102 New Development Pourable Polyamide Thixotrope Conventional Paste Polyamide

BB-102

5Îźm

Electron Microscope Photos

Easily dispersed by post-addition.


DISPARLON BB-102: Anti-sagging in Acrylic-Urethane Formulation Raw material

Parts

Acrydic A-801

60.0

Butyl acetate

5.0

TiO2 CR-93

35.0

Additive

6.0

Hardener / BURNOCK DN-950

18.0

Dispersing condition Dissolver / 4cm blade Speed : 2000 r.p.m. Time : 10 min. Viscosity : 65 KU (stomer)

400μ m 500μ m 600μ m Blank

Conventional

BB-102


K-STAY Attributes ®

• Based on proprietary King Industries sulfonate technology • Designed for use in pigmented solvent borne systems • Highly efficient at low use levels to improve pigment suspension and sag control • Do not detract from gloss • Easy to use – pourable liquids • Highly shear thinning for spray applications • Effective in a wide range of resin systems

Attributes


K-STAY Properties Product

State

Technology

% Solids

Solvent

Availability

K-STAY 501

Liquid

Overbased Sulfonate

50

K-STAY 511

Liquid

Sulfonate

50

K-STAY 555

Liquid

Overbased Sulfonate

IRCOGEL 955

Gell

IRCOGEL 941 IRCOGEL 916

Price $/LB 1-2 Drums

Applications

Aromatic 100

Commerical Limited

$8.50

General purpose Alkyds, acrylics, polyester, epoxy Anti-sag & settle

Aromatic 100

Commercial Unlimited

$5.70

Low viscosity Not efficient in all formulas

57

Aromatic 100 / Mineral Spirits

Scale up Unlimited

$4.87

955 replacement

Overbased Sulfonate

57

Aromatic 100

---

---

General purpose

Liquid

Overbased Sulfonate

40

Aromatic 100

---

---

Liquid version of 955

Liquid

Overbased Sulfonate

54

Aromatic 100

---

---


K-STAY Appearance

K-STAY 501

K-STAY 511

K-STAY 555

IRCOGEL 955


K-STAY Sag Performance Resin: Polymac 5776 (Polyester) Bake Enamel


DISPARLON Thixotropes for Waterborne Coatings •

• • •

Unique high shear thinning associative type rheology modifier Anti-settling with low viscosity Hydrophobic Excellent pigment orientation

Pearlescent pigment : Iriodin 300 Acrylic Melamine System Stored at room temperature for 7 days Viscosity: 180 mPa.S 15 μ 35 μ 55 μ BLANK

BLANK

AQ-600 (2%)

Polyamide (2 %)

BLANK

AQ-600 (3%)


Rheology Modifier Comparison Polyamide

Viscosity

Ρ

Urethane Associative

Acrylic Type Alkali-swellable

Urethane Associative (High ICI Versions)

Blank

Shear Rate

Îł


DISPARLON AQX-60 (Cosolvent free) New Development Viscosity: 30 sec. (F.C.#4) Stored for 1 week at room temp.

Blank

AQX-60

Additive A

Additive B

Blank

AQ-607

AQX-60

Additive A

Additive B

Dosage (Solid %)

0.0

0.4

0.4

0.4

0.4

Vis. [mPa シ s]

19.3

630

600

5390

420

T.I.

1.0

4.6

4.5

1.2

2.1

Additive A : Urethane Type Additive B : Acrylic Type


Advantage of AQH-800 - Easy incorporation Appearance

AQ-600

  AQ-607

  AQ-610

AQH-800

SM/AQH53


DISPARLON AQH-800 - 1K Self Crosslinking Wood Coating ( NeoCryl XK-98 DSM Neo Resins )

Anti-Settling Effect Application vis. : FC#4 27 sec. ( 25℃ )

After 1 week at room temperature

After 1 week at 50℃

SM/AQH54


DISPARLON AQH-800 - 1K Self Crosslinking Wood Coating ( NeoCryl XK-98 DSM Neo Resins )

Anti-Sagging Effect

Blank      

AQH-800    

Acrylic

      Urethane  

Application vis. : FC#4 27 sec. (25℃)

SM/AQH55


DISPARLON AQH-800

- Automotive OEM Primer‐ Surfacer Test formulation Part A Setaqua 6071 AQ-44 W-1

Polyester resin ; Nuplex Resins Barium sulphate ; Takehara Kagaku Kogyo

95.68 29.44

SL-2000 JR-600A MA-100 Water DMEA

Calcium Carbonate; Takehara Kagaku Kogyo Titanium dioxide ; TAYCA Carbon Black ; Mitsubishi Chem.

29.44 58.88 0.44 23.84 0.48 238.20

pH control agent   (pH 8.0)   Paint formulation

Part   A Setaqua 6071 AQ-44 DMEA Water Diethyleneglycol monobutyl ether Setamine MS-152 IB-70 Rheology control agent  

Polyester resin; Nuplex Resins pH control agent (pH 8.0) Co-solvent Melamine resin; Nuplex Resins

238.2 95.68 0.30 31.36 10.08 30.77 α

Sand-mill grinder 2000rpm×60min.

Additive 0.4 % (as active component) Dissolver 1800rpm×15min.

406.39 + α

SM/AQH56


DISPARLON AQH-800

- Automotive OEM Primer‐ Surfacer ( Setaqua 6071 AQ-44 / Setamine MS-152 IB-70 Nuplex Resins )

Test result Dosage (%)

 

Flow curve 1000

Initial Vis.60rpm

AQH-800 Acrylic Urethane Blank

T.I.

Blank

-

1018

1.3

AQH-800

0.4

1201

3.4

Acrylic

0.4

17510

1.6

Urethane

0.4

1987

1.2

viscosity (Pa.s)

100.0

10.00

1.000

Viscosity ; FC#4 26sec. 25℃  

0.1000

Dilution   (%)

Vis.60rpm

T.I.

Blank

6.1

134

1.7

AQH-800

8.9

325

4.4

Acrylic

17.7

192

2.2

Urethane

19.3

124

1.5

Low-High 0.01000 1.000E-3

0.1000

1.000 10.00 shear rate (1/s)

100.0

1000

10000

Viscosity : FC#4 26 sec. (25℃)

SM/AQH57


DISPARLON AQH-800

- Automotive OEM Primer‐ Surfacer ( Setaqua 6071 AQ-44 / Setamine MS-152 IB-70 Nuplex Resins )

Anti-Sagging effect 30μ

40μ

50μ

30μ

Blank   30μ

40μ

Acrylic

40μ

50μ

AQH-800 50μ

30μ

40μ

50μ

Urethane Spray viscosity : FC#4 26 sec. Setting : 20℃ 10min. Baking : 80℃ 10min. → 145℃ 30min.

SM/AQH58


DISPARLON AQH-800

- Automotive OEM Primer‐ Surfacer ( Setaqua 6071 AQ-44 / Setamine MS-152 IB-70 Nuplex Resins )

Anti-Settling Effect Application vis. : FC#4 26 sec. (25℃ )

After 2 weeks at room temperature Blank  

After 2 weeks at 40℃

SM/AQH59

AQH-800

Acrylic

Urethane


DISPARLON AQH-800 - Anti-Settling Agent for Tinter Anti-settling effect of pigment paste After 1 week at room temperature

Blank   AQH-800

AcrylicUrethane

After 1 week at 50℃

Blank   AQH-800 AcrylicUrethane

SM/AQH60


DISPARLON NS-5500 Attributes • Post-addable hybrid type thixotropic agent for SB systems • Excellent pigment orientation of metallic, pearlescent and flattening silica. • Excellent pigment suspension • Ease of use: Pourable liquid • Easy incorporation by post-addition


DISPARLON NS-5500 Performance Blank

5% NS-5500

Hard Pack Anti-settling Test: 7 Days (Viscosity: 17 sec #4 Ford)


DISPARLON NS-5500 Performance Pigment Orientation

Blank

NS-5500


DISPARLON NS-5500 Applications

• Satin & semigloss wood varnishes and coatings • Aerosol coatings • Metal and plastic coatings • Auto OEM and refinish


DISPARLON NS-5500 Properties Appearance

White liquid

% Active

7

Solvent

Aromatic 100, ethanol, IPA

Typical Use Levels: 3.0 to 8.0% based on total formula weight.


DISPARLON AQ-340 & AQ-380 Attributes • Dispersants for WB systems • Designed to disperse carbon black and organic pigments • Excellent color development • Superior efficiency with carbon black • Excellent gloss and hiding power • Easily incorporated


DISPARLON AQ-340 & AQ-380 Performance Formulation of Pigment paste: Vis.(mPa ・ s) [D=19.2s-1]

T.I.

Particle Size (μm)

Blank

Dispersant

EMPEROR

20.0

20.0

Blank

4124.0

6.9

1.26

Water

80.0

72.0

AQ-380

35.2

1.2

0.12

Dispersant

-

16.0

Additive A

1075.0

3.9

0.21

Total

100.0

108.0

Additive B

1188.0

7.7

0.36

Test Result:

20° Gloss

Hiding

Blank

53.8

0

AQ-380

91.4

5

Additive A

81.6

3

Additive B

85.7

3

Blank

AQ-380


DISPARLON AQ-340 & AQ-380 Properties Appearance

Light yellow liquid

% Active

30%

Solvent

Propylene glycol monomethyl ether

Typical Use Levels: • 3 to 30% by weight for inorganic pigments • 40 to 130% for organic pigments


Colorants