IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0594379
(2006-11-08)
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등록번호 |
US-8247072
(2012-08-21)
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발명자
/ 주소 |
- Sumner, Jr., Charles Edwan
- Munjal, Ramesh Chand
- O'Meadhra, Ruairi Seosamh
- Sink, Chester Wayne
- Fauver, Jerry Steven
- Schisla, Jr., Robert Melvin
- Bagrodia, Shriram
- Hochstetler, Spencer Erich
- Hardin, Tera Jill
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출원인 / 주소 |
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
0 인용 특허 :
84 |
초록
Resol beads are disclosed that are prepared in high yield by reaction of a phenol with an aldehyde, with a base as catalyst, a colloidal stabilizer, and optionally a surfactant. The resol beads have a variety of uses, and may be thermally treated and carbonized to obtain activated carbon beads.
대표청구항
▼
1. A process for producing resol beads having a desired particle size and particle size distribution, the process comprising: a) reacting a phenol with an aldehyde, in the presence of a base as catalyst, in an agitated aqueous medium provided with a colloidal stabilizer, and optionally a surfactant,
1. A process for producing resol beads having a desired particle size and particle size distribution, the process comprising: a) reacting a phenol with an aldehyde, in the presence of a base as catalyst, in an agitated aqueous medium provided with a colloidal stabilizer, and optionally a surfactant, for a period of time and at a temperature sufficient to produce an aqueous dispersion of resol beads;b) recovering resol beads below a minimum particle size;c) recycling the previously formed resol beads below the minimum particle size into a further aqueous medium of step a) to give a further aqueous dispersion of resol beads;d) optionally separating any beads below the minimum particle size to obtain resol beads above a minimum particle size and further previously formed resol beads below the minimum particle size; ande) optionally recycling any further previously formed resol beads below said minimum size to step c);wherein the previously formed resol beads are not further cured prior to recycling. 2. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a median particle size from about 10 μm to about 1,500 μm. 3. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a median sphericity value from about 0.90 to 1.0. 4. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a median particle size from 75 μm to 750 μm. 5. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a median particle size from about 125 μm to about 300 μm. 6. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a particle size distribution span from about 10 to about 500. 7. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a particle size distribution span from about 25 to about 250. 8. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a particle size distribution span from about 25 to about 150. 9. The process according to claim 1, wherein the resol beads above the minimum particle size have a median particle size from about 10 μm to about 2,000 μm. 10. The process according to claim 1, wherein the resol beads above the minimum particle size have a median sphericity value from about 0.90 to 1.0. 11. The process according to claim 1, wherein the resol beads above the minimum particle size have a median particle size from about 100 μm to about 750 μm. 12. The process according to claim 1, wherein the phenol comprises monohydroxybenzene. 13. The process according to claim 1, wherein the aldehyde comprises formaldehyde. 14. The process according to claim 1, wherein the base comprises one or more of ammonia or ammonium hydroxide. 15. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) are provided in an amount of at least 10 wt. %, based on the weight of the phenol. 16. The process according to claim 1, wherein the molar ratio of the aldehyde to the phenol is from about 1.1:1 to about 3:1. 17. The process according to claim 1, wherein the colloidal stabilizer comprises a carboxymethyl cellulose salt. 18. The process according to claim 17, wherein the carboxymethyl cellulose salt has a degree of substitution from about 0.6 to about 1.1 and a weight average molecular weight from about 100,000 to about 400,000. 19. The process according to claim 1, wherein the total external surface area of the previously-formed resol beads provided to step c) is at least 4 m2 per each kilogram of phenol. 20. The process according to claim 1, wherein the temperature is from about 70° C. to about 98° C. 21. The process according to claim 1, wherein the temperature is from 75° C. to 90° C. 22. The process according to claim 1, wherein the surfactant is present and comprises an anionic surfactant. 23. The process according to claim 1, wherein the surfactant is present and comprises one or more of: sodium dodecyl sulfate or sodium dodecyl benzene sulfonate. 24. The process according to claim 1, wherein the base comprises one or more of: ammonia or hexamethylenetetramine. 25. The process according to claim 1, wherein the process further comprises adding, after the reacting of step a) has begun, a further portion of a base. 26. The process according to claim 1, wherein the process further comprises adding, after the resol beads of step a) are formed, an acid. 27. The process according to claim 1, wherein methanol is present in the aldehyde provided to the reaction mixture of step a) in an amount of no more than about 2 wt. %, based on the total weight of the aldehyde. 28. The process according to claim 1, wherein the agitated aqueous medium is agitated by one or more of: a pitched blade impeller; a high efficiency impeller; a turbine; an anchor; a spiral agitator; a rotating agitator; a flow induced by circulation; or flowing the aqueous medium past a stationary mixing device. 29. The process according to claim 1, wherein the previously-formed resol beads that are recycled according to step c) have a median particle size from 125 μm to 250 μm and a particle size distribution span from about 25 to about 150, and the resol beads obtained in step c) have a median particle size from 250 μm to 500 μm. 30. The process according to claim 1, wherein the resol beads obtained in step c) comprise from about 0.5% nitrogen to about 3% nitrogen, based on elemental analysis. 31. The process according to claim 1, wherein the resol beads obtained in step c) comprise from 0.8% nitrogen to 2.6%, based on elemental analysis. 32. The process according to claim 1, wherein the previously formed resol beads that are recycled according to step c) are soluble in methanol in an amount up to 20 wt. %. 33. The process according to claim 1, wherein the previously formed resol beads that are recycled according to step c) have a Tg from about 30° C. to about 120° C., as measured by DSC. 34. The process according to claim 1, wherein the previously formed resol beads that are recycled according to step c) have a Tg from 30° C. to 68° C., as measured by DSC. 35. The process according to claim 1, wherein the resol beads obtained in step c) have an acetone solubility of no more than about 5%. 36. The process according to claim 1, wherein the resol beads obtained in step c) have an acetone solubility of no more than 15%. 37. The process according to claim 1, wherein the resol beads obtained in step c) have an acetone solubility of no more than 26%. 38. The process according to claim 1, wherein the resol beads obtained in step c) have an acetone solubility of no more than 30%. 39. The process according to claim 1, wherein the resol beads obtained in step c) have a density from about 0.3 g/mL to about 1.3 g/mL. 40. The process according to claim 1, wherein the resol beads obtained in step c) have a density from 0.5 to 1.3 g/mL.
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