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Pigment
What is pigment
A pigment is a material that changes the color of reflected or transmitted light as the result of wavelength-selective absorption. This physical process differs from fluorescence, phosphorescence, and other forms of luminescence, in which a material emits light Many materials selectively absorb certain wavelengths of light. Materials that humans have chosen and developed for use as pigments usually have special properties that make them ideal for coloring other materials. A pigment must have a high tinting strength relative to the materials it colors. It must be stable in solid form at ambient temperatures.
PIGMENT
is a particulate solid dispersed into a medium without solution or significant interaction
Pigment
Dye
Applications of Pigments
1 2 3 4 5 6 7 8 9 Inks : water and solvent based Paints : water and solvent based Plastics : all types including EVA Rubber Glass Ceramic Textile Cement Products Cosmetics
Color Strength
Full-Tinting Strength
1.
TUJUAN : Untuk memastikan bahwa analisa warna plastik resin PVC dengan two roll mill dilakukan dengan benar
2. RUANG LINGKUP : Instruksi kerja ini menjelaskan cara kerja analisa warna plastik resin PVC dengan two roll mill yang berlaku untuk produk B-201 pengiriman Maspion atau customer lain yang requirment sejenis. 3. BAHAN BAHAN YANG DIPAKAI PVC Soft Natural (Type : EH 1000) TiO2 (Type : Tronox CR-834) DOP (Dioctyl Phthalate) Stabilizer (Methylene Mercaptide) Sample 5. CARA KERJA Pembuatan Compound Timbang bahan untuk bahan untuk campuran compound I dengan komposisi : -. PVC soft = 50gram -. DOP = 5gram -. Stabilizer = 5 gram Kemudian timbang juga bahan untuk bahan untuk campuran compound II dengan komposisi: -. PVC soft = 45 gram -. DOP = 4,5 gram -. Stabilizer= 4,5 gram Buka kran steam ke alat two roll mill yang sudah di set dengan tekanan 2 kg/cm2 untuk mencapai suhu 130C. Set jarak antara two roll mill 0,1 mm dengan fuller dan sesuai tanda batas pada alat. Masukkan bahan compound diatas ke alat two roll mill sambil dilakukan pengadukan. Setelah campuran masuk semua, grinding dan diaduk dengan kape selama 10 menit dengan menjaga besar ukuran compound 5,5 6 cm dari pinggir roll. Compound diangkat dan didinginkan pada suhu ruangan. Dibuat oleh :
TEST METHOD
Pewarnaan Compound I. Timbang sample = 0,0240 gr . Tekanan steam dinaikkan menjadi 2,8 3,0 kg/cm2 sampai suhu two roll mill menjadi 140C Setelah suhu two roll mill mencapai 140C, masukkan compound campuran I lakukan pengadukan sampai homogen. Masukkan campuran sampel / pigment pelan-pelan ke dalam compound campuran I. Setelah sampel masuk semua lakukan penggilingan dengan two roll mill sambil diaduk-aduk selama 5 menit . Kemudian compound hasil pewarnaan diatas, diangkat dan didinginkan pada suhu ruang. Pewarnaan Compound II. 1. Setelah dingin compound hasil pewarnaan I dipotong dan ditimbang = 6,0000 gr ( untuk pewarnaan ke II) Masukkan compound campuran II lakukan pengadukan sampai homogen. Kemudian masukkan compound pewarnaan I yang sudah ditimbang, lakukan penggilingan sambil diadukaduk selama 5 menit. Kemudian compound diangkat dan didinginkan pada suhu ruang. Setelah dingin potong dengan ukuran 3 x 3 cm sebanyak 10 lembar untuk 1 kali press. Pressing Setting alat hot press pada suhu 190C dan diamkan sampai suhu stabil. Mould dibersihkan dan dikeringkan. Taruh potongan compound hasil pewarnaan pada mould dengan standard / pembanding pada posisi keri dan sampel / yang dibandingkan pada posisi kanan. Mould ditutup dan masukkan kedalam hot press. Lakukan pressing dengan tekanan 2,5 Mph suhu 190C selama 3 menit. Selesai pressing keluarkan mould dari hot press kemudian dinginkan dengan cooling press selama 1 menit. Setelah dingin plate dibuka, lihat hasilnya dan ukur warnanya dengan chromameter.
Formulir Instruksi Kerja : FIK I5.1-43021/RX Buku harian Analisa Warna Plastik Resin PVC Dengan Two Roll Mill
Solvent Fastness
Forms of Pigments
Solid
Presscake
Chip, masterbatch
Heat Fastness
Good
Insoluble in sovents Have little degree of solubility May be unsafe Usually safe
Azo Pigments
Azo Pigments have the azo group (-N = N-) There are 2 stages for the synthesis of azo pigments: - Diazonium salt formation - Coupling reaction
REACTOR
REACTOR
FILTER PRESS
Disazo Pigments
Disazo Pigments : 2 classes 1. The coupling of di and tetra substituted diaminodiphenyls with acetoacetic arylides or pyrazolones 2. The coupling of diazotization of aromatic amines with bisacetoaceticarylides 3. These pigments cover the colour range from greeny yellow to reddish yellow & orange & red 4. They have better solvent & migration fastness than mono azo pigments & are use in printing inks & plastic The color potential of disazo pigments covers the color range from very greenish yellow and orange and red
- Naphthol Pigments
Beta Naphthol Pigments provide colours from orange to medium red Production by coupling reaction with beta naphthol
Solvent resistant, migration fastness & light fastness are comparable to mono azo yellow pigments Commercial application in paints
These pigments provide colour from yellowish & medium red to brown & violet
They are obtain by coupling reaction of aryl diazonium salt with aryllides of 2-hydroxy-3-naphthoic acid
Azo Pigment Lake (Salt Type Pigments) These pigments provide colours between medium red to bluish red
They are from by precipitating a monoazo compound with contain sulfo & / or carboxy groups with metal cations such as calcium, barium, magnesium, strontium or manganese. These pigments have limited light fastness & migration resistance but good heat fastness.
Benzimidazolone Pigments
These pigments cover the spectrum from greenish yellow to orange & medium red to maroon
There two type : the first one is obtain by coupling with 5acetoacetylaminobenzymidazolone,the second one the coupling components is 5-2-hydroxy-3-naphthoaylaminobenzymidazolone
Pigment performance including light fastness & weather ability is excellent Application in plastics & hybrid printing inks
They have wood solvent & migration resistance & light fastness Application in plastic & spin dyeing
SYNTHESIS of Isoindolinone
Polycylic Pigments
These are pigments with condendsed aromatic or heterocyclic ring systems They have good light, heat and weather fastness and good solvent and migration resistance They are more expensive than azo pigments except the phthalocyanine pigments They are use in all application ranging from water & solvent base inks, water & solvent base paints, plastic, rubber, cement & textile
Phthalocyanine Pigments
These pigments are the most produced organic pigment in the world. They cover the colour from greenish blue to reddish blue & blueish green to yellowish green They are produce by reacting metal salt with nitrogen source compound & phthalic acid derivative
They show good solvent & migration resistance, good , light, heat, chemical & weather fastness Commercial application cover a whole range of product
Quinacridone Pigments
These pigments available in a reddish violet and a blueish red Like the phthalocyanine pigments ,quinacridone are make in two stages , the preparation of crude quinacridone and the pigmentation the crude They have outstanding light & weather fastness & solvent & migration resistance Commercial application are for high grade coating ( automotive), for plastics & special inks
SYNTHESIS of Perinone
Perinone
Thioindigo Pigments
Anthrapyrimidine Pigments
SYNTHESIS of Anthrapyrimidine
Flavanthrone Pigments
Flavanthrone yellow .the only commercially use flavanthrone is a brilliant reddish yellow
Excellent light and weather fastness combined with good solvent and migration resistance
SYNTHESIS of Flavanthrone
Pyranthrone Pigments
Most pigments are orange but others are blueish red colour
Anthanthrone Pigments
The only commercial pigments is dibromoanthanthrone which provides shade of scarlet for metallic finishes They have outstanding weather fastness Commercial application are in high grade
SYNTHESIS of Anthanthrone
Dioxazine Pigments
These pigments produced violet colouration and in combination with phthalocyanine blue pigment produces a very reddish shade Dioaxazine Pigments are derived from triphenodioxazine, linear system of five anelated rings They show extreemly light and weather fastness as well as excellent solvent and migration resistance Commercial application include the pigmentation of plastics, printing inks, spin dyeing and coating
Triarylcarbonium Pigments
The colour covers from green,violet and victoria blue
There are two types of these pigments: salt of triphenylmethane sulfonic acid salt of heteropolyacid with tungsten, molybdenum, silicon or iron They have poor solvent resistance and limited light fastness but have excellent colour brilliant and clarity of hue better than any other organic and /organic pigments Commercial application is for printing inks especially are for packaging inks
Quinophthalone Pigments
They are mostly greenish yellow These pigments have a polycylic structure derived from quinaldine and phthalic anhydride They have excellent temperatures resistance
The main market for these pigments are in the plastics and coating industries
SYNTHESIS of Quinophthalone
Synthesis of Pigments
Production of CI Pigment Yellow 1, 11680 Diazotization In a vessel 912 kg of 4-methyl-2-nitroaniline is stirred over night with water. Then 3395 L of 5 mol / L HCl is added, together with some ice to lower the temperatures to 0 C. Sodium nitrite solution, 792 L of 40 wt % is then run in underneath the surface. Any excess sodium nitrite is removed by addition of 3- nitro- ptoluidine. Active charcoal is added as clarifying agent and then filtered
Dissolution the coupling component AcetoAcetanilide, 1098kg, is strirred with water for 1 H at 25C then 510 kg of CaCO 3 and 206 kg of 33% NaOH solution is then added.
Coupling The reaction mixture is heated to 33 C and the clarified diazonium salt solution is then run in. After 30 minutes HCl is added to adjust the pH to 3-4. After 20 minutes the pigment is separated by filtering through a filter press and wash with water to remove salt. The filter cake ( press cake ) is dried at 60-65C The yield is 2042 kg
The soln is run into a mixture of 3500 L of water and 1120 L of 5 mol/L of HCl. The reaction mixture is cooled to 0C by addition of ice and repeatedly diazotizide with 185 L of 40 wt %NaN02 soln. The temp must not exceed 0 C.
After 2 h, 107 kg of CaCO3 suspended in water is added, The volume is made up to 28500L with water; active charcoal are added and the soln is filtered thro a clarifying filter.
Dissolution of the coupling component At 30 C, 420 kg of naphthol AS/D is dissolved in 322 L of 33% of NaOH and 3000L of water ; 10 kg of active charcoal is then added and the soln is filtered. The volume is made up to 14000 L and temp is 20 C. Then 84 g of Igepon T in 200 L of water is added and the mixture is cooled to 3 C with ice. The coupling component is precipitated by rapid addition of 235 L of glacial acetic acid. Coupling
The reaction mixture is heated to 38 C, and the filter diazonium salt soln is run in under the surface of the suspension of the coupling component within 3,5 h. After completion of coupling, the pigment is isolated by filtering the suspension thro a press, washing to remove salt and drying at 50-55 C. The yield is 700 kg
In industry, this pigment is produced in two stages The first stage is the preparation of the Blue Crude CuPc while the 2nd is the Pigmentation of crude CuPc ie the reduction of particle size of Crude CuPc.
Crude CuPc is commonly prepared by reacting copper chloride urea, phthalic anhydride, catalyst with solvent.
CuCl + 12 H2NCONH2 + 4 C6H4 (CO)2O (produced in Malaysia) CuPc + NH3 + CO2 + H2O + NH4Cl
Structure of CuPc
Yield 90%
The Phthalocyanine is filtered of ; washed with hot trichlorobenzene at 50 C, methanol and hot water; and dried.
The yield of CuPc is 87 kg
Filter Press
Department
Purchasing QC R&D
Duty
To buy raw materials, machinery, lab equipments, spare parts of machinery and packaging etc To set the standard and control the quality of the raw materials, finish products and packaging To produce new cheap products which satisfy customers requirements based on preliminary research by Technical Support To produce consistent products To find the market for the products and to set the quarterly sale forecast To repair the damage and worn out parts of machinery To research customer complains regarding with quality & packaging problems and to prepare test methods for the finish products suitable for customers and to do preliminary research for new products based on customers requirements
Sand Fiber
Free Copper Content PCB
TM 9 TM 10
TM 11 TM 12
1.
2..
Environmental Effect Most of the waste of the production of crude CuPc (11,000 tons/yr) is precipitated using Na2S and then is buried underground
Pigmentation Process
Methods Pigments Produced Notes Reddish blue pigment with heat stability up to 170 C and poor solvent resistant Reddish blue pigment with heat stability up to 350 C but poor solvent resistant Reddish blue pigment with heat stability up to 350 C and good solvent resistant Dissolving in conc H2SO4 Blue Pigment 15:0 and then sprayed into aqueous solution containing certain additives Blue Pigment 15:1
Grinding with inorganic Blue Pigment 15:3 salts with the aids of polyol solvent in the presence of certain additive in kneader Blue Pigment 15-4 or ball mill
Ball Mill
Pigmentation by Grinding
Production of Beta-CuPc Pigment from Crude CuPc In a kneader , 283kg of crude CuPc is ground for 8 hours with 1131 kg of NaCl and 283 kg of Diethylene Glycol (DEG). Then this paste is boiled in 6000 L of water and filtered using filter press to remove water/soluble substances. Washing with hot water is continued until no water soluble substances can be found.
The presscake is then dried at 70 C 75 C or using spin flash drier. A intensive greenish blue beta-CuPC is obtained.
The yellowish green are obtained with nine to ten bromine atoms per molecule
The Phthalogreens are economical and have good light fastness
The most common organic green pigments are Phthalocyanine green The Phthalogreens are made by halogenating CuPc blue to produce mixtures of CuPc in which many of the 16 hydrogen atoms on CuPc have been replaced by chlorine or mixture of chlorine and bromine atoms The pigments vary from blue green to yellow green depending on the ratios of bromine to chlorine
The yellowish green are obtained with nine to ten bromine atoms per molecule The Phthalogreens are economical and have good light fastness
MARKET DEMAND for Copper Phthalocyanine World production of this product is over 110,000 tons/year while the gap between the world demand and the supply according to Business Analyst for Asahi Songwon Colors Ltd for 2011 is 19,000 tons / year.
PRODUCTION COUNTRIES Crude CuPc was used to be produced in Japan, Europe and America but now it has been shifted to mainly China and India due to lower labor cost and also mainly as the waste regulations of these countries are not strictly followed.
Phthalic anhydride Cuprous Chloride Urea Ammonium molybdate CuPc (just raw materials cost) FOB Price of CuPc (from Baiyan China)
$ 3,517 / MT
$ 5,760 /MT
CALCULATIONS
Material Weight used for 1 MT CuPc 191 kg Unit Price / MT Cost
CuCl
$ 6,565
$ 1,254.00
Phthalic Anhydride
Urea Catalyst Total Cost CuPc
1143 kg
1390 kg 2.60 kg
$ 1,500
$ 350 $ 24,000
$ 1,714.50
$ 487.00 $ 62.40 $ 3,517.90 / MT
Profit
The profit for the manufacturers of this product would increase tremendously by using this new process. For example, a medium size manufacturer that produces 5000 MT CuPc/ year with the FOB price of the low quality CuPc is $5.76/kg, the expenses are as follow:
If the cost of raw materials ($3.52), packaging ($0.04) and energy ($0.44) to be $4.00/kg then to produce 5000 MT = $20m
And if the cost for machinery is assumed to be $1m so a 5 yrs depreciation= $0.2m/yr And if the number of workers employed is 100 with salary assumed to be $600/month each, so salary = $0.72m/yr
Profit
Then Profit :
(5000 MT x $5.76) - $20m - $0.2m - $0.72m + (10% x 5000 MT x $5.76) = $7.88m + $2.88m $10.76m/yr (before depreciation of building, Interest & Tax) The profit should be more than this as the saving cost for the waste treatment should be added to this amount.