zinc;prop-2-enoate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: An equivalent of zinc carbonate was added to acrylic acid in dilute solution to obtain a solution of zinc acrylate. From this solution and other ingredients, there was prepared an aqueous solution containing 1% acrylic acid, 0.9% zinc carbonate, 0.25% MBA, 8% DMDHEU, 2% polyethylene softener, 0.1% wetting agent, and 0.5% K2S2O8. Cotton printcloth was impregnated in this reagent solution to a wet pickup of approximately 105%. The wet fabric was placed on pin frames in heat-resistant plastic bags that were flushed with nitrogen. The samples of fabrics in the bags were subjected to heating in forced-draft ovens at 120° C for 10 minutes, immediately followed by 160° C for 5 minutes. The samples of fabric were washed extensively in hot running tap water and line dried. The weight gain due to add-on of reagent was 7.1%; the nitrogen incorporated into the fabric was 0.88% and the zinc incorporated was 0.39%. The DP appearance rating was 3.1. Textile properties are summarized in Table I and antibacterial properties are summarized in Table III.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In this experiment, acrylic acid was reacted with zinc carbonate to form zinc acrylate prior to addition of the other components. The reagent systems was prepared to contain 8% acrylic acid, 6.9% zinc carbonate, 0.25% MBA, 8% DMDHEU, 2% polyethylene softener, 0.1% wetting agent, and 0.5% K2S2O8. Samples of fabric that were impregnated with this reagent solution to wet pickups of approximately 110% were placed on pin frames in heat-resistant plastic bags that were flushed with nitrogen and sealed. In these bags, fabrics were subjected to 3 different curing conditions: (a) 120° C for 10 minutes followed 160° C for 5 minutes, (b) 120° C for 10 minutes followed by removal from bag and 160° C for 5 minutes, and (c) at 160° C for 15 minutes. The samples of fabric were rinsed extensively in hot-running tap water and line dried. Weight increases due to reaction of reagents were (a) 22.2%, (b) 23.6%, and (c) 21.7%; the DP appearance ratings for these 3 samples were 4.2, 4.5, and 4.3, respectively. The textile performance properties are summarized in Table I. In all three cases attractive levels of resilience and Accelerotor abrasion resistance were obtained. Sample (a) was tested and found to be 100% effective against S. epidermidis in the modified Quinn test.

Conditions: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 4000 liter jacketed stainless steel reactor, at room temperature, were fed successively toluene (1472 kg), zinc oxide (310 kg, 99% purity, 3.77 kmol) and stearic acid (56.0 kg, 0.197 kmol). Then, the temperature was raised to 55±5° C. To the reactor was added dropwise acrylic acid (506 kg, 7.02 kmol) over 2.5 hours, and continued the stirring while keeping at this temperature for additional 2 hours in order to complete the reaction. To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8, comprising mainly polyoxyethylene alkyl ether). After stirring for additional 30 minutes, the resulting cream-like mixture was fed into a paddle dryer for distilling off toluene and water under reduced pressure, and pulverizing the powder. A modified zinc acrylate as a white fine powder was thus obtained (780 kg, 96.7% yield). Moisture content is<0.5 wt %, acryl content is 56.1 wt % and an analyzed ash content is 38 wt %. IR spectrum (KBr): λ 2917, 2848, 1644, 1575, 1522, 1447, 1433, 1373, 1365, 1274, 1067, 974 cm−1. After discharging the material, no cluster stuck on the blade in the dryer was observed, and no cake was detected in the powder. at room temperature the reaction To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8 for distilling off toluene and water under reduced pressure

Conditions: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 4000 liter jacketed stainless steel reactor, at room temperature, were fed successively toluene (1472 kg), zinc oxide (310 kg, 99% purity, 3.77 kmol) and stearic acid (56.0 kg, 0.197 kmol). Then, the temperature was raised to 55±5° C. To the reactor was added dropwise acrylic acid (506 kg, 7.02 kmol) over 2.5 hours, and continued the stirring while keeping at this temperature for additional 2 hours in order to complete the reaction. To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8, comprising mainly polyoxyethylene alkyl ether). After stirring for additional 30 minutes, the resulting cream-like mixture was fed into a paddle dryer for distilling off toluene and water under reduced pressure, and pulverizing the powder. A modified zinc acrylate as a white fine powder was thus obtained (780 kg, 96.7% yield). Moisture content is<0.5 wt %, acryl content is 56.1 wt % and an analyzed ash content is 38 wt %. IR spectrum (KBr): λ 2917, 2848, 1644, 1575, 1522, 1447, 1433, 1373, 1365, 1274, 1067, 974 cm−1. After discharging the material, no cluster stuck on the blade in the dryer was observed, and no cake was detected in the powder. at room temperature the reaction To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8 for distilling off toluene and water under reduced pressure

Conditions: temp:55.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 4000 liter jacketed stainless steel reactor, at room temperature, were fed successively toluene (1472 kg), zinc oxide (366 kg, 99% purity, 4.41 kmol) and stearic acid (65.1 kg, 0.23 kmol). Then, the temperature was raised to 55±5° C. To the reactor was added dropwise acrylic acid (587 kg, 8.15 kmol) over 2.5 hours, and continued the stirring while keeping at this temperature for additional 2 hours in order to complete the reaction. To this reaction mixture was added Sinopol 1807 (2.0 kg, HLB 10.7, comprising mainly polyoxyethylene octadecyl ether). After stirring for additional 30 minutes, the resulting cream-like mixture was fed into a paddle dryer for distilling off toluene and water under reduced pressure, and pulverizing the powder. A modified zinc acrylate as a white fine powder was thus obtained (910 kg, 96.5% yield). Moisture content<0.5 wt %, acryl content is 55 wt % and ash content is 39 wt %. IR spectrum (KBr): λ 2917, 2848, 1644, 1576, 1522, 1447, 1433, 1373, 1274, 1067, 974 cm−1. After discharging the material, no cluster stuck on the blade in the dryer was observed, and no cake was detected in the powder. at room temperature the reaction To this reaction mixture was added Sinopol 1807 (2.0 kg, HLB 10.7 for distilling off toluene and water under reduced pressure

Conditions: temp:48.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 4000 liter jacketed stainless steel reactor, at room temperature, were fed toluene (1591 kg, moisture content of 3.7%), zinc oxide (403.0 kg, 94.5% purity, 4.68 kmol) and stearic acid (65.7 kg, 0.23 kmol). Then, the temperature was raised to 48±5° C. To the reactor was added dropwise acrylic acid (631 kg, 8.76 kmol) over 2.5 hours, and continued the stirring while keeping at this temperature for additional 2 hours in order to complete the reaction. The pH value of this solution is about 5. To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8, comprising mainly polyoxyethylene octadecyl ether). After stirring for additional 30 minutes, the resulting cream-like mixture was fed into a paddle dryer for distilling off toluene and water under reduced pressure, and pulverizing the powder. A modified zinc acrylate as a white fine powder was thus obtained (947.8 kg, 94.6% yield). Moisture content<0.5 wt %, acryl content is 52 wt % and ash content is 36.3 wt %, IR spectrum (KBr): λ 2917, 2848, 1651, 1603, 1537, 1443, 1372, 1276, 1069, 983 cm−1. 99% of its particles have a particle size of<44 μm as shown in the following data determined by a particle size analyzer (model FRITSCH PARTICLE SIZER ANALYSETTE 22) over the range of 0.31 μm to 44.85 μm: at room temperature the reaction To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8 for distilling off toluene and water under reduced pressure

Conditions: temp:48.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a 4000 liter jacketed stainless steel reactor, at room temperature, were fed toluene (1591 kg, moisture content of 3.7%), zinc oxide (403.0 kg, 94.5% purity, 4.68 kmol) and stearic acid (65.7 kg, 0.23 kmol). Then, the temperature was raised to 48±5° C. To the reactor was added dropwise acrylic acid (631 kg, 8.76 kmol) over 2.5 hours, and continued the stirring while keeping at this temperature for additional 2 hours in order to complete the reaction. The pH value of this solution is about 5. To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8, comprising mainly polyoxyethylene octadecyl ether). After stirring for additional 30 minutes, the resulting cream-like mixture was fed into a paddle dryer for distilling off toluene and water under reduced pressure, and pulverizing the powder. A modified zinc acrylate as a white fine powder was thus obtained (947.8 kg, 94.6% yield). Moisture content<0.5 wt %, acryl content is 52 wt % and ash content is 36.3 wt %, IR spectrum (KBr): λ 2917, 2848, 1651, 1603, 1537, 1443, 1372, 1276, 1069, 983 cm−1. 99% of its particles have a particle size of<44 μm as shown in the following data determined by a particle size analyzer (model FRITSCH PARTICLE SIZER ANALYSETTE 22) over the range of 0.31 μm to 44.85 μm: at room temperature the reaction To this reaction mixture was added Sinopol 1536 (2.0 kg, HLB 12.8 for distilling off toluene and water under reduced pressure

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: U.S. Pat. No. 5,789,616 disclosed a process comprising adding at the first an anionic surfactant, sodium dioctyl sulfosuccinate, in toluene, following with adding successively zinc oxide, fatty acid and acrylic acid, and, after completion of the reaction, drying by distillation at a reduced pressure, and pulverizing and sieving the thus produced crude product to yield a modified zinc acrylate powder having a particle size characterized in that 64% of particles<44 μm, 54% of particles<10 μm, and 41% of particles<5 μm, while the part that had a particle size of>105 μm and must be removed by sieving was estimated to be 31%. The anionic surfactant, i.e. sodium dicotyl sulfosuccinate, used in this technique to be added at the first stage of the reaction might cause the swelling of the content in the reaction mixture such that in the subsequent addition of acrylic acid, might lead to local thickening and hence difficulty for stirring, and therefore, the reaction could be completely only through slow addition of raw material and postponing the reaction time. This might be the cause that made the zinc acrylate powder thus produced coarser and the particle size distributions non-uniform. On the other hand, it had an advantage that the trouble of sticking the wall of the reactor and the drying tank in the course of drying could be avoided. after completion of the reaction drying by distillation at a reduced pressure sieving the thus produced crude product

Conditions: temp:15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a jacketed kneader made of SUS-316, 10 liters in inner volume, 5,926 g of toluene as an organic solvent and 11.4 g of sodium dioctyl sulfosuccinate (produced by Kao Co., Ltd. and marketed under trademark designation of "Pellex OT-P") as an anionic surfactant were placed, then 1,411 g of zinc oxide was added thereto and stirred to be suspended therein and, with the internal temperature of the kneader kept at 40° C., a solution of 540 g of stearic acid as a higher fatty acid in 1,809 g of toluene was added to the stirred suspension over a period of one hour, and the suspension and the added solution were left reacting for 2 hours. Then, the internal temperature of the kneader was cooled to 15° C. and 2,362 g of acrylic acid was added to the reaction mixture therein gradually over a period of 3 hours so as to elevate the temperature to 35° C. and they were left reacting at 40° C. for 4 hours. The reaction mixture was gradually heated to 50° C. under a reduced pressure so as to allow the pressure to reach 20 Torrs and effect the expulsion of the water formed by the reaction and toluene by distillation over a period of 5 hours and obtain 3,988 g of zinc acrylate containing zinc stearate. kept at 40° C. the suspension and the added solution were left gradually over a period of 3 hours so as to elevate the temperature to 35° C. and they were left reacting at 40° C. for 4 hours The reaction mixture was gradually heated to 50° C. under a reduced pressure so as

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: An equivalent of zinc carbonate was added to acrylic acid in dilute solution to obtain a solution of zinc acrylate. From this solution and other ingredients, there was prepared an aqueous solution containing 1% acrylic acid, 0.9% zinc carbonate, 0.25% MBA, 8% DMDHEU, 2% polyethylene softener, 0.1% wetting agent, and 0.5% K2S2O8. Cotton printcloth was impregnated in this reagent solution to a wet pickup of approximately 105%. The wet fabric was placed on pin frames in heat-resistant plastic bags that were flushed with nitrogen. The samples of fabrics in the bags were subjected to heating in forced-draft ovens at 120° C for 10 minutes, immediately followed by 160° C for 5 minutes. The samples of fabric were washed extensively in hot running tap water and line dried. The weight gain due to add-on of reagent was 7.1%; the nitrogen incorporated into the fabric was 0.88% and the zinc incorporated was 0.39%. The DP appearance rating was 3.1. Textile properties are summarized in Table I and antibacterial properties are summarized in Table III.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: An equivalent of zinc carbonate was added to acrylic acid in dilute solution to obtain a solution of zinc acrylate. From this solution and other ingredients, there was prepared an aqueous solution containing 1% acrylic acid, 0.9% zinc carbonate, 0.25% MBA, 8% DMDHEU, 2% polyethylene softener, 0.1% wetting agent, and 0.5% K2S2O8. Cotton printcloth was impregnated in this reagent solution to a wet pickup of approximately 105%. The wet fabric was placed on pin frames in heat-resistant plastic bags that were flushed with nitrogen. The samples of fabrics in the bags were subjected to heating in forced-draft ovens at 120° C for 10 minutes, immediately followed by 160° C for 5 minutes. The samples of fabric were washed extensively in hot running tap water and line dried. The weight gain due to add-on of reagent was 7.1%; the nitrogen incorporated into the fabric was 0.88% and the zinc incorporated was 0.39%. The DP appearance rating was 3.1. Textile properties are summarized in Table I and antibacterial properties are summarized in Table III.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In this experiment, acrylic acid was reacted with zinc carbonate to form zinc acrylate prior to addition of the other components. The reagent systems was prepared to contain 8% acrylic acid, 6.9% zinc carbonate, 0.25% MBA, 8% DMDHEU, 2% polyethylene softener, 0.1% wetting agent, and 0.5% K2S2O8. Samples of fabric that were impregnated with this reagent solution to wet pickups of approximately 110% were placed on pin frames in heat-resistant plastic bags that were flushed with nitrogen and sealed. In these bags, fabrics were subjected to 3 different curing conditions: (a) 120° C for 10 minutes followed 160° C for 5 minutes, (b) 120° C for 10 minutes followed by removal from bag and 160° C for 5 minutes, and (c) at 160° C for 15 minutes. The samples of fabric were rinsed extensively in hot-running tap water and line dried. Weight increases due to reaction of reagents were (a) 22.2%, (b) 23.6%, and (c) 21.7%; the DP appearance ratings for these 3 samples were 4.2, 4.5, and 4.3, respectively. The textile performance properties are summarized in Table I. In all three cases attractive levels of resilience and Accelerotor abrasion resistance were obtained. Sample (a) was tested and found to be 100% effective against S. epidermidis in the modified Quinn test.