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  Anion adsorbing carbon material, as well as manufacturing method and manufacturing facilities for sameUSPTO Application #: 20070123420Title: Anion adsorbing carbon material, as well as manufacturing method and manufacturing facilities for same Abstract: This invention provides an anion adsorbing carbon material which is inexpensive, environmentally friendly and excellent in the anion adsorption, as well as a manufacturing method and a manufacturing facilities for the same. This invention is characterized in that a raw material which comprises plant(s) is contacted with a solution including calcium ions, and after that, carbonized, and subsequently, contacted with an acid solution. (end of abstract) Agent: Snell & Wilmer LLP (oc) - Costa Mesa, CA, US Inventors: Satoshi Hayashi, Riei Yokoyama USPTO Applicaton #: 20070123420 - Class: 502417000 (USPTO) Related Patent Categories: Catalyst, Solid Sorbent, Or Support Therefor: Product Or Process Of Making, Solid Sorbent, Free Carbon Containing, And Specified Adde Active Sorbent Material The Patent Description & Claims data below is from USPTO Patent Application 20070123420. Brief Patent Description - Full Patent Description - Patent Application Claims
TECHNICAL FIELD [0001] This invention relates to an anion adsorption carbon material for adsorbing anions such as nitrate ions and fluoride ions, as well as a manufacturing method and a manufacturing facilities for the same. BACKGROUND ART [0002] Contamination of a water quality and soil by heavy metals, agricultural chemicals and an organochlorine compounds has become a problem in that it destroys the environment. Though these harmful substances can be adsorbed and removed with adsorbents such as activated carbon and a zeolite, it is presently difficult to treat nitrate nitrogen, nitrite nitrogen, fluorine, arsenic and cyan which exist in the form of anions with adsorbents. [0003] That is to say, nitrate nitrogen and nitrite nitrogen are included in fertilizers used in tea fields, turfs for golfing and the like, and have become a factor in ground water contamination, which is presently a large problem. This is because nitrate ions and nitrite ions have negative charge and do not become insoluble salt by combining with other chemical substances, and therefore, very easily washes out from negatively charged soil. Thus, though measures against the above described problem are r there are limitations, such that anaerobic conditions are required in biological treatment where, for example, denitrifying bacteria are used to remove nitrate ions and nitrite ions, and in addition, there are similar limitations with other methods, and no effective measures have been found. On top of this, recently, it has come to be believed that nitrate nitrogen and nitrite nitrogen are environmental hormones. [0004] In addition, fluorine is included in wastewater from semiconductor factories, glass factories, plating factories and the like, and though a method for adding calcium compounds to fluorine in industrial wastewater so that the fluorine can be removed in the form of calcium fluorine is used, further installation of adsorption towers having an anion exchange resin for active alumina and fluorine is required, raising the cost. In addition, expensive dedicated anion exchange resins are required in order to meet the Japanese environmental standard of 0.8 mg/L. Furthermore, expensive anion exchange resins are separately required for treating arsenic, cyan and the like, which are included in industrial wastewater and ground water. [0005] As described above, no inexpensive material for adsorbing anions including nitrate ions as that described above have been found at present, and therefore, contamination by these anions tends to sped, and once the environment is contaminated by anions as described above, high cost becomes necessary to restore it. [0006] Patent Document 1: Japanese Unexamined Patent Publication H10 (1998)-165824 DISCLOSURE OF THE INVENTION [0006] Problem to be Solved by the Invention [0007] Therefore, inexpensive and environmentally friendly anion adsorbing materials have been sought. Though charcoal, which is a representative porous material, together with activated carbon, is widely used as a humidity controller, liver purifier and soil conditioner, and is used for removing chlorine based gases and sulfur oxides in waste gas, for example, it simply uses the adsorptive properties of micro pores inside porous carbon materials, in the same manner as activated carbon, and nitrate nitrogen, nitrite nitrogen, fluorine, arsenic, cyan and the like which exist in the form of anions are barely absorbed. [0008] This invention is provided taking the above described situation into consideration, and an object thereof is to provide an anion adsorbing carbon material which is inexpensive, environmentally friendly and excellent in the anion adsorption, as well as a manufacturing method and a manufacturing facilities for the same. Means for Solving the Problem [0009] Then present inventors examined the anion absorbing performance of a material gained by contacting a solution including calcium ions (it is desirable for calcium ions to be included mainly as cations), for example, a solution (lime water) or suspension (milk of lime) of a calcium hydroxide with a raw material which comprises plant(s), in advance, that is, before carbonizing this material, so that Ca (calcium) is introduced into this material, after that, carbonizing this material into which Ca has been introduced and contacting the gained charcoal into which Ca has been introduced with an acid such as HCl, H.sub.2SO.sub.4 or the like, and as a result, found that the material had excellent anion adsorption ability. In addition, in this case, wastewater is treated simply by neutralizing the acid, which is environmentally friendly. [0010] As the solution including calcium ions, a calcium acetate solution, a calcium chloride solution and the like can be cited, in addition to lime water and milk of lime, and a solution including 0.03 weight % to 30 weight % of calcium, preferably 0.1 weight % to 7.0 weight %, is appropriate. [0011] As the method for contacting the solution including calcium ions with the above described material originating from plant(s), dripping, application, spraying, atnizng or the like of the solution including calcium ions is possible, and immersion of the above described material in the solution including calcium ions is most efficient. In addition, as the method for contacting the acid solution with the carbonized material, dripping, application, spraying, atomizing or the like of the acid solution is possible, and immersion of the carbonized material in the acid solution is most efficient. [0012] Thus, a manufacturing method for an anion adsorbing carbon material according to claim 1 is characterized in that a raw material which comprises plant(s) is contacted with a solution including calcium ions, and after that, carbonized, and subsequently, contacted with an acid solution. [0013] In addition, a manufacturing method for an anion adsorbing carbon material according to claim 2, that is, another aspect of the invention, is characterized in that a raw material which comprises plant(s) with which a solution including calcium ions have contacted is carbonized and the carbonized material is contacted with an acid solution. [0014] Furthermore, a manufacturing method for an anion adsorbing carbon material according to claim 3, that is, still another aspect of the invention, is characterized in that a carbonized material gained by carbonizing a raw material which comprises plant(s) with which a solution including calcium ions have contacted is contacted with an acid solution. [0015] As the material originating from plant(s) in this invention, though any plant can be applied, a material of one or more from among natural fibers and ligneous materials, which makes the carbonized material of the above described material porous, is desirable, and any type of ligneous material, such as thinning, lumber and waste wood, as well as natural fibers such as hemp, can be cited as examples. In the case where a solution (for example, lime water or milk of lime) barely including anions (for example, chloride ions) that can be ion exchanged with anions that are the object of adsorption and including calcium ions is used as the solution with which the above described material is contacted, it is desirable for the above described material to be a material where innumerable particles of a calcium compound having a diameter of no greater than 100 nm are formed in the micro pores of a carbonized material when the material is carbonized after calcium has been introduced, and concretely, it is preferable to use ligneous chips of a size of no greater than 10 mm gained by processing a conifer, such as Japanese cypress or cedar having high water absorbency. [0016] In addition, in the case where a solution (for example, a calcium chloride solution) including both anions (for example, chloride ions) which can be ion exchanged with anions that are the object of adsorption and calcium ions is used, it is desirable for the solution to easily soak into the above described material when the material is immersed in the solution, and concretely, it is preferable to use ligneous chips of a size of no greater than 50 mm gained by processing a conifer, such as Japanese cypress or cedar having high water absorbency. Furthermore, whichever solution is used, bamboo, sawdust, chaff, coconut palm, betel-nut palm, jute and straw can be used as the material originating from plant(s). In addition to these, agricultural waste, such as peels and pulp from mandarin oranges and apples, can be cited as the above described material originating from plant(s). In addition, the portion of plants having conductive tissue (vessels, tracheids and sieve tubes) are particularly preferable as the material originating from plant(s). [0017] In this invention, a solution including calcium ions, for example, lime water or milk of lime, contacts with a raw material which comprises plant(s). When the above described material is immersed in the solution including calcium ions, the solution soaks into the material, and thereby, chips into which Ca has been introduced can be gained. In particular, in the case where an alkali solution (for ample, lime water) is used as the solution including calcium ions, as shown in FIG. 7(A), ligneous chips 2, which are an example of a raw material which comprises plant(s), can be immersed in and is contacted with lime water C, so that chips 30 into which Ca has been induced [see FIG. 7(C)] can be gained, and this is considered to be because, as shown in FIG. 7(B), organic matter in ligneous chips 2 is dissolved in alkali, and calcium ions react with a certain component of ligneous chips 2. Here, it is preferable for the solution including calcium ions to contain 0.03 weight % to 30 weight % of calcium, and it is more preferable for it to contain 0.1 weight % to 7.0 weight %. [0018] Next, in this invention, the gained chips 30 into which Ca has been introduced as described above [see FIG. 8(A)] are carbonized, and thereby, charcoal 31 into which Ca has been introduced (hereinafter simply referred to as Ca charcoal) is gained [see FIG. 8(C)], and it is considered that at this point during carbonization, organic matter in chips 30 into which Ca has been introduced [see FIG. 8(B)] decomposes due to heat, and at the same time, calcium ions deposit on the surface of the walls of micro pores in chips 30 into which Ca has been introduced [see FIG. 8(C)]. In this case, calcium ions deposit on the surface of the walls of micro pores in chips 30 into which Ca has been introduced [see FIG. 8(B)], and this is considered to be because calcium ions become of a microscopic and highly dispersed state, and thereby, many functional groups are drawn out from every corner in the walls of the micro pores. [0019] In this invention, a raw material which comprises plant(s) which has been contacted with a solution including calcium ions is carbonized, and after that, an acid solution contacts with this carbonized material, and thereby, functional groups which have been drawn out form the walls of micro pores in the carbonized material are combined with anions which can be ion exchanged with anions that are the object of adsorption. As a result of diligent research, the present inventors found that more functional groups of the carbonized material can be generated during the process of carbonization by controlling the temperature and the time. [0020] That is to say, the present inventors confirmed that in the case where calcium has contacted with a material as that described above in advance, as in the invention according to claim 1, and the material is cooled naturally after the temperature for carbonization of 650.degree. C. to 750.degree. C. has been maintained for, for example, one hour, more functional groups can be formed, in comparison with the case where the material is cooled naturally after the temperature for carbonization of approximately 600.degree. C. or approximately 800.degree. C. has been maintained for one hour. In particular, when a material was contacted with a calcium and carbonized at a temperature for carbonization of 650.degree. C. to 750.degree. C. as described above, and observed through an electron microscope, a state where microscopic particles of the calcium compound half deposited on the surface of walls of the micro pores as described above and were uniformly dispersed was observed. Continue reading... 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