Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Acrylic Acid | HCID 6581 | — |
| Reactant | 2-Isocyanatoethyl methacrylate | HCID 35409 | — |
| Reactant | L-Ascorbic Acid | HCID 54670067 | — |
| Solvent | Water | HCID 962 | — |
| Product | Acrylic Acid | HCID 6581 | — |
| Product | Methylenebisacrylamide | HCID 8041 | — |
Reaction Steps
In a 500 ml four-necked flask equipped with a stirrer, a thermometer, a reflux condenser, a dropping funnel and a nitrogen gas introducing device, 5 g of polysuccinimide obtained in Synthetic Example 2 and 10 g of DMF were charged and dissolved at about 60° C., and then 0.25 g of 2-methacryloyloxyethyl isocyanate was added. As a result, heat was generated. After the reaction was continued for 30 minutes, the temperature in the system was reduced to about 35° C., 1 g of a pregelatinized starch was charged. After the atmosphere in the four-necked flask was replaced by a nitrogen gas, 7.5 mg of 2,2-azobisaminodipropane dihydrochloride, 5 mg of ascorbic acid and 57 mg of an aqueous hydrogen peroxide (35%) solution were respectively dissolved in 1 g of ion exchange water. The resulting solutions were added to the above aqueous solution, and then the mixture was heated to about 60° C. and maintained for three hours ((1) first step). To the polymer obtained by this step, 25 g of acrylic acid and 25 mg of N,N′-methylenebisacrylamide were added. After the atmosphere in the four-necked flask was replaced by a nitrogen gas, 7.5 g of 2,2-azobisaminodipropane dihydrochloride, 5 mg of ascorbic acid and 57 mg of an aqueous hydrogen peroxide (35%) solution were respectively dissolved again in 1 g of ion exchange water. The resulting solutions were added to the above aqueous solution in this sequence, and then the mixture was heated again to about 60° C. and maintained at the same temperature for three hours ((1) second step). 1.2 g of hexamethylenediamine was dissolved in 20 g of ion exchange water and the resulting solution was added to the above aqueous solution, and then the reaction was conducted. Furthermore, 10.4 g of sodium hydroxide was dissolved in 30 g of ion exchange water and the resulting solution was added, thereby to neutralize carboxyl groups originating in acrylic acid ((1) third step). The resulting gel-like product was dried at 110° C. by a vacuum drier and the resulting dry solid was ground to obtain a water absorbent material of the present invention. The evaluation results of characteristics of the resulting water absorbent material are shown in Table 2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06969750B2 |
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| Source dataset | uspto-grants-2005_11 |
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| ORD ID | ord-dfa2d8970ada4eaebb3d9828f4b10f05 |
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| Source note | uspto-grants-2005_11 |
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