Autophoretic 866

Alex Plant Development

Date 19/10/2010 www.autophoretic.net

Created By

Mr.Khaled El-Deeb Autophoretic /Aquence Consultant

khaled@autophoretic.net Tel:-+2019.3000.833 /+2010.886.7714

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Introduction:-

The AUTOPHORETIC coating process has been in commercial use since 1973. Since then, continuing development of new latex polymers in the 1980's has led to greatly improved appearance, performance and ease of use, and has greatly expanded the applications for the process. The increasing emphasis on environmental issues has also made autodeposition a very attractive process because of its lack of organic solvents. Since 1986, over 30 production lines have been installed using AUTOPHORETIC coating chemicals to coat parts as diverse as small brackets to full automotive leaf spring assemblies. Process Description Both Nano-Ceramic and ACC866 process could be used on the same production line so that its called dual technology process production line.

work package
(work package capacity =21 scissors =21m)

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Process Sequence

Stage No
1 2 3 4 5 6 7 8 9 10 11 12 13 14

Description
Alkaline Clean Degreasing Plant Water Rinse Hcl Picking Plant Water Rinse Neutralization Plant Water Rinse D.I Water Rinse Nano-Ceramic DI or R.O. Water Rinse
Autophoretic 800, Coating Plant Water Rinse Reaction Rinse 2150 Curing

Comment
Spray Immersion Immersion Immersion Immersion Immersion Immersion Immersion Closed Closed Immersion Immersion Immersion Oven (one Zone)

(Production capacity = 42 scissors/h)

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Warning
Before starting in nano-Ceramic Process ensure that you closed the ACC coating Bathes (11-12-13) with good cover

Before starting in The ACC coating Process ensure that you closed the nano-Ceramic Bathes (9-10) with a good cover

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Stage No (1) Hot Spray Alkaline Cleaning

Overview

1 2 3 4 5 6 7

Purpose Room Dimensions (cm) Tools Chemicals content Temperature C Concentration Pressure Width Length Height

Pre Cleaning 305 380 300 Karcher Machine ,items rack Progal D 346 TF ,Ridosol Operating parameters 75-90 C 2-3% Pa

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Stage No (2) Degreasing Bath

Tank overview

1 2 3 4 5 6 7 8 9

Purpose Width Length Bath Dimensions (cm) Height Volume Materials of construction Agitation method Chemicals content Temperature C Concentration Reference Mark ml Immersion time

Degreasing 240 120 100 2.88m Mild steel Thermally isolated Pump with Eductors Progal D 346 TF ,Ridosol Operating parameters 70-95 C 30-100 g/l 4.6-6.6 ml 5-20 min Based on oil/wax rust level

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Control Sheet (Degreasing Bath )

Bath Volume =2.88m

Build-up
Chemical
1 2 3 Progal D 346 TF Ridosol Deionized Water

Quantity
144 kg 14 L 2733 L

Use a separate drum to dissolve the Progal D completely in hot D.I water then transfer it into your tank Add ridosol directly to your tank in three period 4 L /H Leave the tank to be agitate for one hour Check up the Operation parameter Start in production

Note
For a new bath adjusted to 50 g/l , this reference mark should be approx. 5.6 ml

Operation
Reference Mark : Time Temperature Application : : : 4.6 - 6.6 ml 5 - 20 min 70 - 95C Immersion

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TESTING AND CONTROL (Degreasing

Never pipette by mouth, use a pipette filler.

Bath )

The Progal D 346 TF bath is controlled in the plant by the reference mark (FA)

Method
1-pipette a sample of exactly 10 ml from the bath into 250 ml conical flask 2-dilute with 100 ml D.I water 3-add few drops of indicator # 3 homogenize the solution 4-The sample will turn pink 5-Using the 25 ml burette filled to the 0 mark with titration solution 27 6-titrate the sample until the pink coloration disappears 7-Record the number of ml of titration solution 27 used which represent the reference mark

Note
-For a new bath adjusted to 50 g/l , this reference mark should be approx. 5.6 ml -keep the concentration within 5.6 1 ml -for subsequent titrations add 25.6 kg of progal D 346 TF to the bath per point below reference mark

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Stage No (3) Plant water Rinse Bath

Tank overview

1 2

Purpose Bath Dimensions (cm) Width Length Height Volume

3 4 5 6 7 8 9

Materials of construction Agitation method Chemicals content Temperature C Reference Mark Conductivity Immersion time

Tap water Rinsing 240 120 100 2.88m Mild Steel inside of the bath be shot blasted and coated with a good quality 2K epoxy paint Air agitation Tap Water Operating parameters ambient 0.46-0.66 ml 400 s 60 Sec

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Control point (Tap water Rinse Bath )

Bath Volume =2.88m

Build-up
Chemical
1 Tap Water

Conductivity
200s

Operation
Conductivity : 400s 0.46-0.66 ml 60 Sec ambient Immersion

Reference Mark : Time Temperature Application : : :

TESTING AND CONTROL(Tap

water Rinse Bath )

This rinsing bath controlled by two parameter . bath conductivity and Reference mark -Conductivity measurement

Kindly follow up your instrument manual for . Electrode cleaning , and calibration

Use your appropriate conductivity meter for direct measuring conductivity value

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-Reference mark measurement

Never pipette by mouth, use a pipette filler. The water rinse bath is controlled in the plant by the reference mark FA to determine the amount of Degreasing chemicals escaped to the water rinse so that we are going to use the same degreasing control process .

Method
1-pipette a sample of exactly 10 ml from the bath into 250 ml conical flask 2-dilute with 100 ml D.I water 3-add few drops of indicator # 3 homogenize the solution 4-The sample will turn pink 5-Using the 25 ml burette filled to the 0 mark with titration solution 27 6-titrate the sample until the pink coloration disappears 7-Record the number of ml of titration solution 27 used which represent the reference mark

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Stage No(4) Pickling Bath

Tank overview

1 2

Purpose

3 4 5 6 7 9

Pickling Width 240 Length 120 Bath Dimensions (cm) Height 100 Volume 2.88m Mild Steel Materials of construction Lined by polypropylene OR good Quality anti acid Fiber Agitation method Air agitation Chemicals content Hcl Operating parameters Temperature C ambient Concentration 60-80% by volume Immersion time 5-10 min Based on the rust and corrosion level

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CONTROL METHOD Pickling Bath

Transfer 5 mls of the bath solution to a 250ml beaker by means of a safety pipette. Dilute with approximately 100ml of distilled water. Place the probe of a suitably calibrated pH meter into the solution and titrate against 1N. Sodium Hydroxide until pH 3.8 is reached. (Care must be taken during titration after pH 2.0 is reached as beyond this point the pH changes very quickly with small additions of the titrant) Note burette reading - this is the titration value. Record this Value to be your reference mark

IRON VALUE The point at which the solution should be discarded is reached when the iron content exceeds 70 grams per litre. The method of determining the iron content is as follows: Transfer 2 mls of the solution to a 150 ml flask by means of a safety pipette. Dilute with approximately 50 ml of distilled water; carefully add 5 ml of concentrated Phosphoric Acid, followed by 3 drops of diphenylamine indicator solution. Titrate against N/10 Potassium Dichromate solution until a violet blue colour is produced. 1 ml of N/10 Potassium Dichromate is equivalent to 0.0056 grams of iron - therefore, 70 grams/litre of iron will give a titration value of 25.0 mls N/10 Potassium Dichromate per 2 ml sample.

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Stage No(5) Plant water Rinse Bath

Tank overview

1 2

Purpose Bath Dimensions (cm) Width Length Height Volume

3 4 5 6 7 8

Materials of construction Agitation method Chemicals content Temperature C Conductivity Immersion time

Tap water Rinsing 240 120 100 2.88m Mild Steel lined with fiber OR inside of the bath be shot blasted and coated with a good quality anti acid 2K epoxy paint Air agitation Tap Water Operating parameters ambient 400 s 60 Sec

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Stage No (6) Neutralization Bath

Tank overview

1 2 3 4 5 6 7 8 9

Purpose

Degreasing Width 240 Length 120 Bath Dimensions (cm) Height 100 Volume 2.88m Materials of construction Mild steel Thermally isolated Agitation method Pump with Eductors Chemicals content Progal D 346 TF ,Ridosol Operating parameters Temperature C 70-75 C Concentration 30-100 g/l FA ml 4.6-6.6 ml Immersion time 5 min

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Control Sheet (Neutralization Bath )

Bath Volume =2.88m

Build-up
Chemical
1 2 3 Progal D 346 TF Ridosol Deionized Water

Quantity
144 kg 3L 2880 L

Use a separate drum to dissolve the progal completely in hot D.I water then transfer it into your tank Add ridosol directly to your tank in three period 1 L /H Leave the tank agitation for one hour then start in production

Operation
Reference Mark : Time Temperature Application : : : 4.6 - 6.6 ml 5 - 20 min 70 - 95C Immersion

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TESTING AND CONTROL(Neutralization Bath )

Never pipette by mouth, use a pipette filler. The Progal D 346 TF bath is controlled in the plant by the reference mark FA

Method
1-pipette a sample of exactly 10 ml from the bath into 250 ml conical flask 2-dilute with 100 ml D.I water 3-add few drops of indicator # 3 homogenize the solution 4-The sample will turn pink 5-Using the 25 ml burette filled to the 0 mark with titration solution 27 6-titrate the sample until the pink coloration disappears 7-Record the number of ml of titration solution 27 used which represent the reference mark

Note
-For a new bath adjusted to 50 g/l , this reference mark should be approx. 5.6 ml -keep the concentration within 5.6 1 ml -for subsequent titrations add 25.6 kg of progal D 346 TF to the bath per point below reference mark
References -International training manual (Henkel ACC) -Progal D 346 TF technical data sheet

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Stage No (7) Plant water Rinse Bath

Tank overview

1 2

Purpose Bath Dimensions (cm) Width Length Height Volume

3 4 5 6 7 8 9

Materials of construction Agitation method Chemicals content Temperature C Reference Mark Conductivity Immersion time

Tap water Rinsing 240 120 100 2.88m Mild Steel inside of the bath be shot blasted and coated with a good quality 2K epoxy paint Air agitation Tap Water Operating parameters ambient 0.46-0.66 ml 400 s 60 Sec

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Control point (Tap water Rinse Bath )

Bath Volume =2.88m

Build-up
Chemical
1 Tap Water

Conductivity
200s

Operation
Conductivity : 400s 0.46-0.66 ml 60 Sec ambient Immersion

Reference Mark : Time Temperature Application : : :

TESTING AND CONTROL(Tap

water Rinse Bath )

This rinsing bath controlled by two parameter . bath conductivity and Reference mark -Conductivity measurement

Kindly follow up your instrument manual for . Electrode cleaning , and calibration

Use your appropriate conductivity meter for direct measuring conductivity value

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-Reference mark measurement Never pipette by mouth, use a pipette filler. The water rinse bath is controlled in the plant by the reference mark FA to determine the amount of Degreasing chemicals escaped to the water rinse so that we are going to use the same degreasing control process .

Method
1-pipette a sample of exactly 10 ml from the bath into 250 ml conical flask 2-dilute with 100 ml D.I water 3-add few drops of indicator # 3 homogenize the solution 4-The sample will turn pink 5-Using the 25 ml burette filled to the 0 mark with titration solution 27 6-titrate the sample until the pink coloration disappears 7-Record the number of ml of titration solution 27 used which represent the reference mark

References -International training manual (Henkel ACC)

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Stage No(8) D.I Bath

Tank overview

1 2

Purpose

3 4 5 6 7 8

D.I Rinsing Width 240 Length 120 Bath Dimensions (cm) Height 100 Volume 2.88m Mild steel Lined with fiber with polyester Materials of construction or Stainless Steel Agitation method Air agitation Chemicals content D.I Water Operating parameters Temperature C ambient Conductivity 50s Immersion time 60 Sec

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Control point (D.I Bath )

Bath Volume =2.88m

Build-up
Chemical
1 Deionized Water

Conductivity
5-10 s

Operation
Conductivity : Time Temperature Application : : : 50s 60 Sec ambient Immersion

TESTING AND CONTROL

Kindly follow up your instrument manual for . Electrode cleaning , and calibration

Use your appropriate conductivity meter for direct measuring conductivity value

References -International training manual (Henkel ACC) -Design Manual (Henkel )

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Stages No (9), (10) Nano-Ceramic and D.I Bathes

Both have to be closed

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Stage No(11) Autophoretic866 Coating Bath

Tank overview

Black Coating Width 320 Length 160 Bath Dimensions 2 (cm) Height 160 Volume 8.192 m 3 Materials of construction Mild steel lined with fiber with polyester 4 Agitation method 4 Mixers with 2 fan each connected to VFD 5 Temperature control tools Schaller +heater with coil and hot/cold D.I water 6 Chemicals content ACC866 Rpl , HF , H2O2 , FeF3 , D.I Operating parameters 7 Temperature C 20-22 C 8 Solid content % 5-7 % 9 101 ( F - activity ) A 125-300 10 ORP mV 350-400 11 Starter level ml 27-36 12 Immersion time 90

Purpose

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Control Sheet (ACC866 Bath )

Bath Volume =8.192m

Build-up
Chemical
1 2 3 4 5 AUTOPHORETIC 866 Replenisher Deionized Water AUTOPHORETIC 300 Starter AUTOPHORETIC 35 Activator AUTOPHORETIC 24 Oxidizer

Quantity
1097.7 kg ( 925.7 L ) 6856.7 L 434.2 kg ( 409.6 L ) 30 L 20 L

Build-up technique
Add one to two inches of deionized water to the tank. For each 100 litres of final bath volume, add 13.4 kg (11.3 litres) of AUTOPHORETIC 866 while adding deionized water and mix thoroughly without generating any foam. While mixing, add more deionized water to bring the volume to three-fourths full. Now add 5.3 kg (5 litres) of AUTOPHORETIC 300 Starter per 100 litres of bath. Finally, add sufficient water to bring the solution up to the operating level. Allow bath to agitate for approximately 2 hours and check all bath parameters. Add Oxidizer, Activator or Replenisher as necessary to adjust levels.

Operation
Redox Value Fluoride Meter Reading Total Solids Starter Titration Temperature Time : 375 25 mV 125 to 300 micro amperes 5.0 - 7.0% 36 ml, maximum 20 - 22C 1.5 minutes 20 - 22C Immersion

Temperature : Application :

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TESTING AND CONTROL (ACC866 Coating Bath)

Never pipette by mouth, use a pipette filler. The AUTOPHORETIC 866 bath is controlled in the plant by a Redox Control measurement a Fluoride meter measurement, a Total Solids determination and a Starter Titration.

Redox Control
1-Pick up your ACC866 sample in a 200ml plastic biker 2- clean up your Electrodes with D.I water 3-put the Electrodes in the sample

4-turn on your mV instrument 5-Wait for reading stability 6-Record your ORP value

Kindly follow up your instrument manual for . Electrode cleaning , storage solution and calibration

7-Remove the electrodes from the sample and clean it up 8-turn off the mV 9-Put the electrodes into the storage solution The redox potential is constantly monitored with an appropriate instrument and electrodes. The specification value is maintained by additions of AUTOPHORETIC 24 Oxidizer. The frequency of additions is dependent on the amount of work being processed per unit time and bath volume. Should it be necessary to add AUTOPHORETIC 24 Oxidizer manually, add 0.4 litres per 100 square metres of metal processed. AUTOPHORETIC 24 Oxidizer should be slowly added to maintain the redox potential within the specified range of operation. Our Representative will recommend appropriate equipment required.

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101 Fluoride Meter Reading

Kindly follow up your instrument manual for . Electrode cleaning , storage solution and calibration

1- Rinse and fill sample cup on the 101 D meter with bath. 2- Press Start Timer button. 3- The meter will time itself for 6 minutes, during which time the yellow Timing light will blink. 4- At the end of 6 minutes, the yellow light will become constant and the green Timer Finished light will also be lit. The reading on the digital display will freeze, write down this number as the 101 value.

A Fluoride meter reading is made every 2 hours.. The specification value is maintained by additions of AUTOPHORETIC 35 Activator. The frequency of additions is dependent on the amount of work being processed per unit time and bath volume. The Fluoride meter reading should be maintained within the specified limits. To raise the reading by about 100 microamperes, add 32 liters of AUTOPHORETIC 35 Activator. Our Representative should be consulted for appropriate equipment recommendations and operating instructions.

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Total Solids

Kindly follow up your instrument manual for . calibration

The solids content is measured daily by the following method : a) On a balance capable of weighing to 1.0 milligrams, weigh a small sample dish. Record the weight of the sample dish. To the sample dish add about 3 ml of bath sample. Quickly re weigh the sample dish with the bath sample. Record the measurement Place the sample dish with bath into an oven set at 100C for 60 minutes. Remove the dish and allow to cool to room temperature. Re weigh the sample and record the value Calculate the % total solids : weight of dry sample = B-A x 100 = % Total Solids weight of wet sample C-A A = weight of sample dish B = weight of dry sample and sample dish C = weight of wet sample and sample dish g) Run 2 tests by the above method and average the results.

b) c) d)

e) f)

To raise the Total Solids level 0.1%, add 18.84 litres of AUTOPHORETIC 866.

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Starter titration

The Starter Titration is performed on a shift basis. The value is obtained by the following method : 1- Place a 10 ml sample of coating bath into flask. 2- Add 25 ml of ATS 32 (50 % HCl) 3- Under the hood, heat and boil solution for 1 minute. 4- Dilute with DI water to approximately 100 ml. 5- Cool Solution to room Temperature. 6- Add ATS 35, 1 ml at a time. Solution will go from the present yellow to clear then to a light salmon color. Note: After solution turns clear, add ATS 35 slowly. Generally, 10 to 20 ml of ATS 35 is needed for the color change. 7- Add approximately 1 ml of RS 22. This will cause the solution to turn deep purple. 8- Stir solution and let sit for 1 minute. 9- Titrate with TS 86 (0.01 M EDTA) until the solution changes from purple to a faint orange to a light yellow. Titrate slowly after solution becomes faint orange. 10- Record mils of TS 86 used.

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Testing Reagents:

Composition in order of Addition

Auxiliary Solution 32 (1000g): 460g Deionized Water 540g HCL-37%, AR, ACS

Reagent Solution 22 (1000g): 606,07g Isopropyl alcohol, purified plus 160,0 g Salicylic Acid, 99% 233,93g DI Water

Titrating Solution 86 (1000g): 600g DI Water 3,7g Disodium EDTA, 2H2O

396.3g DI Water

Auxiliary Test Solution 35 (1000g): 350g DI Water 650g Ammonium Acetate crystals-tech

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Check Sheet (ACC866 Bath )

Check point 1 2 3 4 5 6 7 8 1 2 3 4 5 1 2 3 4 5 6 7 8 12 Temperature C Solid content % Rpl add (L) 101 ( F ) A HF add (L) ORP mV H2O2 add (L) Starter level ml Temperature C 101 ( F ) A HF add (L) ORP mV H2O2 add (L) Temperature C 101 ( F ) A HF add (L) ORP mV H2O2 add (L) Total area (m) Part NO Stabilization Note Date
Op. Range

/2010

/2010

/2010

/2010

2010

20-22 5-7 125-300 350-400 34 20-22 125-300 350-400

20-22 125-300 350-400

Don or N

Lab Manager Name :.... Signature :-

Quality Dept Name :.... Signature :-

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Stage No(12) Plant water Rinse Bath

Tank overview

1 2

Purpose

3 4 5 6 7 8

Tap water Rinsing Width 240 Length 120 Bath Dimensions (cm) Height 100 Volume 2.88m Mild Steel inside of the Materials of construction bath be shot blasted and coated with a good quality 2K epoxy paint Agitation method Two mixers connected to VFD Chemicals content Tap Water Operating parameters Temperature C ambient Conductivity 400 s Immersion time 60 Sec

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Control point (Tap water Rinse Bath )

Bath Volume =2.88m

Build-up
Chemical
1 Tap Water

Conductivity
200s

Operation
Conductivity : Time Temperature Application : : : 400s 60 Sec ambient Immersion

TESTING AND CONTROL

Kindly follow up your instrument manual for . Electrode cleaning , and calibration

Use your appropriate conductivity meter for direct measuring conductivity value

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Stage No(13) R.R 2150 Bath

Tank overview

1 2 3 4 5 6 7 8

Purpose

Reaction Rinsing Width 320 Length 130 Bath Dimensions (cm) Height 160 Volume 6.656 m Materials of construction Mild steel lined with fiber with polyester OR stainless Agitation method 2 Mixers with 1 fan each connected to VFD Chemicals content Reaction Rinse 2150 Operating parameters Temperature C ambient 1000-3000 Functional conductivity m mhos m mhos Immersion time 60

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Control Sheet (R.R 2150 Bath )

Bath Volume =6.656m

Build-up
Chemical
1 2 AUTOPHORETIC 2150 Reaction Rinse Deionized Water

Quantity
100 L 6556L

Operation
Functional conductivity Time : 1000-3000 mmhos 60 Sec ambient - 27C Immersion

Temperature : Application :

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TESTING AND CONTROL(R.R

2150 Bath )

Never pipette by mouth, use a pipette filler. The AUTOPHORETIC 2150 bath is controlled in the plant by the functional conductivity

Kindly follow up your instrument manual for . Electrode cleaning , and calibration

1. Determine the conductivity of the ACC 2150 RR processing bath by following the instructions for using your specific type of meter. Record the value obtained , Total Conductivity. 2. Measure 50 ml of bath into a graduated cylinder. 3. Transfer bath into a 250 ml Erlenmeyer flask. 4. Heat solution to a boil and continue to boil for 15 minutes. 5. Cool and transfer liquid contents to a graduated cylinder. Wash the flask several times with small amounts of DI water. Transfer water into graduated cylinder. 6. Bring the volume in the graduated cylinder to the 50 ml mark with DI water. 7. 8. Determine the conductivity of this solution. The conductivity value determined in step 7 above represents the contamination level in the bath. Subtract the value in step 7 from the value obtained in step 1. This represents the Functional Conductivity.

9.

To increased conductivity value 100 mmhos add 6.65 L R.R 2150 to the bath

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Stage No(14) Curing Oven

Overview

1 3 6 7 8

Purpose Temperature prop Temperature C T in prop reading Curing time

Curing 6 prop distributed as shown in fig connected to one reader interface Operating parameters 100-115 C 2 30 min

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Check Sheet
Stage (1) Spray Clean (2) Dip Clean (3) Water Rinse (4) Pickling Hcl (5) Water Rinse

Parameter Pressure Temperature Temperature R.M Additions Conductivity R.M ml R.M ml Iron value Conductivity Temperature

Date Op. Range 75-90 C 70-95 C 4.6-6.6 ml < 400s 0.46-0.66 ml 70 g/l < 400S 70-95 C 4.6-6.6 ml 0.46-0.66 ml < 400s < 50s

Month-year day day

(6) R.M ml Neutralization (7) Water Rinse (8) D.I Rinse

Additions R.M Conductivity Conductivity

(9) ACC866 Coating

ORP - 1 ORP - 2 350-400 mV ORP - 3 101 - 1 101 - 2 125-300 A 101 - 3 Starter Titr. < 36ml % Solids 5.0-7.0 % Bath Cond.s 2500-3500 Temperature 20-22 C Repl. Addition Stabilization Conductivity Func. Cond. mmhos Additions Temperature < 400s 1,000-3,000 mmoh 100-115 C

(10) Water Rinse (11) R.R 2150 (12) Curing

Total Production in 1m

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References
-Autophoretic International training manual (Henkel ACC) -Autophoretic Design Manual (Henkel ) -Progal D 346 TF technical data sheet -Autophoretic 866 technical data sheet

-Autophoretic R.R 2150 technical data sheet

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