______________________________________
Time after dispersion
Percent --NCO
______________________________________
Immediately 100
15 min15 59.6
30 min30 57.2
45 min45 63.2
60 min60 55.3
T.sup.120 - 120 min
27.5
______________________________________
The data indicate that the reaction rate, for this reaction, is fastest in the first fifteen minutes (a 40% decrease in --NCO) and then levels off during the remainder of the first hour (with an additional 5% decrease). The data also indicate that without any other treatment other than the increase in temperature to 60° C., the mole percent of --NCO functionality could only be reduced to 27.5% after two hours.
Example II. After dispersion of the prepolymer, the temperature was brought to 60° C. within 15 minutes. Based on the rate of reaction observed in Example I, the quenching agent, 2.05 g of a 10% by weight solution of NH4 OH (equivalent to 2.2 mol % of unreacted diisocyanate) was added one hour after the dispersion of the prepolymer with mild agitation. The mole percent relative residual --NCO at the reported time intervals are the following:
______________________________________
Time after dispersion
Percent --NCO
______________________________________
Immediately 100
60 min, post-add NH.sub.4 OH
25.9
75 min, 15 min after NH.sub.4 OH
31.2
90 min, 30 min after NH.sub.4 OH
19.1
T.sup.105 - 105 min, 45 min after NH.sub.4 OH
12.2
T.sup.120 - 120 min, 60 min after NH.sub.4 OH
10.0
T.sup.180 - 180 min, 120 min after NH.sub.4 OH
6.8
______________________________________
These data indicate that after two hours the mole percent of residual --NCO functionality could be brought to 6.8%.
Example III. After dispersion of the prepolymer, the temperature was brought to 60° C. within 15 minutes. One hour after the dispersion of the prepolymer, 5.83 g of a 27% weight solution of IPDA (equivalent to 7 mole percent of unreacted diisocyanate) was added with mild agitation. The mole percent relative residual --NCO at the reported time intervals are the following:
______________________________________
Time after dispersion
Percent --NCO
______________________________________
Immediately 100
60 min, post-add IPDA
53.7
75 min, 15 min after IPDA
35.1
90 min, 30 min after IPDA
21.2
T.sup.105 - 105 min, 45 min after IPDA
8.8
T.sup.120 - 120 min, 60 min after IPDA
4.4
______________________________________
Example IV. Thirty minutes after dispersion of the prepolymer, 5.83 g of a 27% weight solution of IDPA was added with mild agitation. The temperature was raised to 60° C. at 60 minutes after dispersion and held at that temperature for 30 minutes. The mole percent relative residual --NCO at the reported time intervals are the following:
______________________________________
Time after dispersion
Percent --NCO
______________________________________
Immediately 100
T.sup.15 - 15 min 82.3
T.sup.30 - 30 min, post-add IDPA,
68.2
temperature at 35° C.
T.sup.45 - 45 min, 15 min after IPDA
42.4
T.sup.60 - 60 min, 30 min after IPDA,
29.9
temperature raised to 60° C.
T.sup.75 - 75 min, 45 min after IPDA
21.9
T.sup.90 - 90 min, 60 min after IPDA
11.4
______________________________________
Example V. Sixty minutes after dispersion of the prepolymer, 5.83 g of a 27% weight solution of IDPA was added with mild agitation. The temperature was raised to 60° C. at 90 minutes after dispersion and held at that temperature for 60 minutes. The mole percent relative residual --NCO at the reported time intervals are the following:
______________________________________
Time after dispersion
Percent --NCO
______________________________________
Immediately 100
15 min15 88.2
30 min, temp at 27° C.
82.3
45 min45 72.4
60 min, post-add IPDA
69.3
75 min, 15 min after IPDA
63.9
90 min, 30 min after IPDA,
58.2
temperature raised to 60° C.
T.sup.105 - 105 min, 45 min after IPDA
24.1
T.sup.120 - 120 min, 60 min after IPDA
14.9
T.sup.135 - 135 min, 75 min after IPDA
12.2
T.sup.150 - 150 min, 90 min after IPDA
3.0
______________________________________
The results of Examples I through III show that there is a substantial percentage of residual --NCO even two hours after the initial dispersing of room temperature water. In contrast, quenching with NH4 OH resulted in only 6.8% residual --NCO three hours after the initial dispersing and two hours after the addition of the NH4 OH, and quenching with IPDA resulted in only 4.4% residual --NCO two hours after the initial dispersing and one hour after the addition of the IPDA.
Examples IV and V show that the rate of decrease in the residual --NCO level is dependent not only on quenching but on an increase in reaction temperature after the dispersion of the prepolymer.
Example VI. The same prepolymer made in the previous examples was made on an industrial scale and dispersed with 25° C. water. The dispersion was made by adding 897 Kg ( lbs) of water to 495 Kg ( lbs) of prepolymer at 60° C. (140° F.). Three samples were drawn off from the reactor and stored in 208 L (55 gal) drums after being treated according to the following procedure:
After dispersion, the reactor contents were held at 38° C. (100° F.) for one hour. A 202 Kg (445 lbs) sample was drawn off into a closed head drum (Drum #1) equipped with a pressure gauge and a relief valve (156 KPa)(8 psig).
To the remaining reactor contents, 19.5 Kg (43 lbs) of a 1.7 weight percent ammonia solution were added in one shot. The reactor contents were held at 38° C. (100° F.) for 15 minutes. A 202 Kg (445 lbs) sample was drawn off into a closed head drum (Drum #2) equipped with a pressure gauge and a relief valve.
The temperature of the remaining reactor contents was increased to 65° C. (about 150° F.) and held at that temperature for 30 minutes. (Level of foam began to increase at this temperature.) The reactor contents were cooled to 38° C. (100° F.), and a 202 Kg (445 lbs) sample was drawn off into a closed head drum (Drum #3) equipped with a pressure gauge and a relief valve.
The same prepolymer made for the previous drum samples was made in a separate industrial scale batch (60° C., 140° F.) and dispersed with 25° C. water. The temperature of the resulting dispersion equilibrated to 38° C., and then sufficient ammonia solution was added to bring the concentration of ammonia in the reactor to 0.023 weight percent (equivalent to 6.6 mol % of unreacted diisocyanate). The reactor contents were heated to 60° C. (140° F.) and sufficient deaerator (Dee Fo , Ultra Additives of Paterson, N.J.) was added to bring the concentration of deaerator to 0.05 weight percent. The reactor contents were cooled to 60° C. (100° F.), and a 202 Kg (445 lbs) sample was drawn off into a closed head drum (Drum #4).
The pressure in each drum was observed every hour. If the pressure of the drum exceeded 135 KPa (5 psig) the gas in the drum was released until the pressure dropped to 101 KPa (0 psig). When the pressure was at the level of 115 KPa (2 psig), the drum visibly bulged. The number of times the pressure was released in 48 hours was recorded, the lower the number, the more effective the procedure for reducing the evolution of CO2 gas.
The physical characteristics of the polyurethane dispersions, the number of pressure releases in 48 hours, and the drum pressure at the end of two weeks are reported here.
______________________________________
Drum #1 Drum #2 Drum #3 Drum #4
______________________________________
% Solids 34.1 33.5 33.2 31.0
Particle 113 110 79 77
size nm
Grit (200)*
0. 0. 0. 0.
% by weight
Grit (325)*
not not 0. 0.
% by weight
tested tested
pH 7.4 7.2 7.4 7.14
Viscosity
14 12 22 18
mPa · s
# Pressure
10 5 0 not
Releases/48 hrs recorded
Pressure ( )
2.5 2.0 less than
no
at 2 weeks gauge bulge
______________________________________
*The grit was caught on a 200 or 325 mesh screen.
Example VII. In separate industrial scale batches, the same prepolymer made in the previous examples was prepared and treated with ammonia or with ammonia and deaerator as described in Example VI. The process conditions, process time, and presence of pressure in the storage drums are recorded here. The record shows that the process time is considerably shortened when the inventive procedure is followed and that there is no pressure build-up on storage (in 208 L, 55 gal drums). In the following table, weight percent values are based on the total weight of the dispersion, and mole percent values are given per mole of unreacted diisocyanate in the prepolymer.
______________________________________
Process Batch Batch Batch Batch
Conditions
#1 #2 #3 #4
______________________________________
Dispersion
(140° F.)
(100° F.)
(100° F.)
(100° F.)
Temperature
60° C.
37.5° C.
37.5° C.
37.5° C.
Ammonia 0 wt % 0 wt % 0.023 wt %
0.023 wt %
0 mol % 0 mol % 6.6 mol %
6.6 mol %
Deaerator
0 0 0 0.05
Wt percent
Foam level
excessive moderate moderate slight
Process time
10.5 11.5 13.75 8.5
in hours
Description
bulging bulging slight no
of Drums bulging bulging
______________________________________
In the field of aqueous-based polyurethanes, [POLYURETHANE DISPERSIONS], we are perhaps the pioneers in India, that complete the chain of Manufacturing the PUDs, from the designing and synthesis of the backbone polyol, to the finished product customized for end use application. We are focused on serving our customers, with a close partnership and delivering world class products. Made in India. like: Aliphatic Single Pack Self Cross Linking Water Borne Polyurethane Dispersion.
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PU Dispersions: This water based solution coatings comprise specialty products ranging from soft to hard, from anionic to cationic, from normal to highly resistant to hydrolysis, from soft to scratch-resistant, from hydrophobic to hydrophilic, from non-swelling to breathable PU polyurethane dispersion a tough balancing act today for coating formulators and end users. Increasingly stringent environmental regulations call for low-VOC products, but one still has to meet the technical requirements for the coating for a variety of substrates. Polyurethane dispersions water borne based coatings are an alternative approach to producing polyurethane coatings and adhesives that are low in VOCs.
PUDS are used in a variety of technical and industrial applications, such as Industrial/Auto and Decorative coatings, wood coatings, leather and PVC leather, adhesives, inks, plastic etc. These products have an ever growing and vast sphere of application. Our products are constantly analyzed and updated to optimize and enhance polymer properties for specific applications, ranging from abrasion resistance to softness of hand. Please find your industry sector and select from the Bansal Trading Company product range the chemicals we can supply. Please consult our sales or technical representative for helpful advice.
SELF CROSS-LINKING
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SUPERIOR ADHESION TO A WIDE VARIETY OF SUBSTRATES
CYCLOALIPHATIC POLYURETHANE
GOOD WEATHER ABILITY
GOOD GLOSS RETENTION
SINGLE PACK
PACKING COST IS REDUCED
PLASTIC CANS CAN BE USED
WATER BASED
LOW VOC
LOW ODOUR
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FREE FROM INSTABILITY IN COST OF SOLVENTS
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MADE IN INDIA
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NO TRANSPORTATION/IMPORT DUTIES ON WATER
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LESS STOCKS AND FASTER DELIVERIES
SAND THE WOOD WITH 120 EMERY PAPER
DILUTE AE- (SANDING SEALER) WITH 10% DI-MINERALISED WATER
APPLY A THIN COAT OF THIS DILUTED AE- SEALER
ALLOW IT TO DRY FOR 4 HOURS AT 20 ° C, OR IF TEMPERATURE IS LOW, DRY OVERNIGHT
SAND THE COATED WOOD WITH 220 EMERY PAPER
APPLY SECOND COAT OF SANDING SEALER DILUTED AE- (PROCEDURE 3 AND 4)
SAND THE COATED WOOD WITH 320 EMERY PAPER
APPLY THIRD COAT OF SANDING SEALER DILUTED AE- (PROCEDURE 3 AND 4)
SAND THE COATED WOOD WITH 600 EMERY PAPER
TOP COAT
FOR GLOSS TOP COAT AE- (DILUTE WITH 10% DI-MINERALISED WATER)
FOR MATT TOP COAT AE- (DILUTE WITH 10% DI-MINERALISED WATER)
APPLY FINAL TOP COAT OF AE- (GLOSS COAT) OR AE- (MATT COAT)
ALLOW IT TO DRY
FOR GLOSS FINISH
SAND THE COATED WOOD WITH EMERY PAPER, AFTER 48 HOURS
BUFF THE COATED WOOD WITH 3M PROTECT IT 1 STEP POLISH
MATT FINISH-NO FURTHER STEPS