Organic compounds -- part of the class 532-570 series – Organic compounds – Halogen containing
Reexamination Certificate
2002-06-26
2004-06-01
Richter, Johann R. (Department: 1621)
Organic compounds -- part of the class 532-570 series
Organic compounds
Halogen containing
C570S140000, C570S142000, C570S153000, C570S175000, C570S177000
Reexamination Certificate
active
06743957
ABSTRACT:
FIELD OF THE INVENTION
Present invention relates to a treatment process reducing a burden to environment and ecosystem about a solution containing a molecular anion having a per-fluorocarbon chain as a main component and a polymer containing fluorine. In addition, it is preferable that said treatment process recovers the above-mentioned anion to use effectively. Specifically, the present invention relates to a technology, which forms a layered double hydroxide to fix the molecular anion having the per-fluorocarbon chain as a main component and the polymer containing fluorine in the solution, and recovers to reproduce these anions preferably.
BACKGROUND OF THE INVENTION
An anion surface-active agent having the per-fluorocarbon chain as a main component is used as an indispensable material of a production process in many fields, such as an emulsion polymerization process of PTFE (poly-tetra-fluoro-ethylene) and a production process of an electronic parts industry. Moreover, said anion surface-active agent is also widely used as a material, which are various paints, a coating agent, and a fire-extinguishing agent, etc. However, in these production processes, the above-mentioned anion surface-active agent has been used as a dilute solution, such as several % to 0.01% by weight. Especially, for example, in the emulsion polymerization of PTFE, a lot of fine particles of PTFE resins to the fluorine anion surface-active agent have suspended in a solution, so that the efficient fixing and recovering on an industrial scale has been difficult. Moreover, the problem of this fixing and recovering has not been considered in general because this solution is dilute. Furthermore, the fluorine compound, such as said anion surface-active agent, is a hard material to be processed by the activated sludge processing, which has been widely used as a wastewater processing. However, a harmony of chemical materials to environment or ecosystem is required strongly in recent years, and, also about this fluorine compound, it is started that the necessity of the technology about the closing system by fixing, recovering and reproducing is recognized strongly.
According to the fixing and recovering of this anion surface-active agent, the technology using the layered double hydroxide has been examined to be in practical use about a phosphate anion or an organic anion, as a scavenger or a removal agent of anions. However, about molecular anion having the per-fluorocarbon chain as a main component, such examinations have not been done previously. In addition, as a conventional technology, it is known that the process, in which an ammonium salt of fluoroalkane acid is extracted to recover by using an organic solvent, such as dichloro-methane or trichloro-methane, was proposed (Japanese Patent Raid Open No. Shou 61-215346), but this process uses an organic solvent containing chlorine, so that it is not enough for reducing the burden to environment. Moreover, by this process, it is necessary to remove the fine particles of PTFE, which are suspended in the solution, so that the processing takes time and effort Furthermore, although it is also known that the other process was proposed, in which fluoroalkane acid was recovered by an ion exchange (WO99/62858, UK1314607), it is also necessary to remove the fine particles of PTFE beforehand in this process.
In addition, the inventors have already reported the layered double hydroxide having anion between layers (Zn
2
Al(OH)
6
C
7
F
15
CO
2
) for the purpose of a material synthesis (the 76th spring annual meeting of the Chemical Society of Japan), about a high concentration aqueous solution of per-fluoro-octanoic acid ammonium (about 8.6% by weight). However, this report was not for the purpose of fixing and recovering of the anion like this invention, about the solution having the wide concentration range including the dilute solution of 0.1% by weight. Therefore, the process about absorbing or fixing of such fluorine compound has not been reported yet.
[Disclosure of the Invention]
Present invention provides the treatment technology, about the solution containing the fluorine compound having the per-fluorocarbon chain and the polymer containing fluorine, in which the layered double hydroxide having the fluorine compound is formed to precipitate with the polymer containing fluorine simultaneously. In addition, it is preferable that said treatment technology fixing to recover efficiently the anion having the per-fluorocarbon chain as the main component, such as carboxylic acid ion, sulfonic acid ion, etc., from the aqueous solution having the wide concentration range including the dilute aqueous solution of 0.1% by weight.
That is, this invention provides the process comprising the following constitutions.
[1] A treatment process of a solution containing an organic compound having a fluorocarbon chain (hereinafter said to as the fluorine compound) and a polymer containing fluorine, the process comprising,
adding divalent and trivalent metal salts to said solution,
forming a layered double hydroxide having the fluorine compound between layers to fix the fluorine compound, and
precipitating said layered double hydroxide with the polymer containing fluorine.
[2] A treatment process of a solution containing the fluorine compound and a polymer containing fluorine, the process comprising,
adding divalent and trivalent metal salts to said solution,
forming a layered double hydroxide having the fluorine compound between layers to fix the fluorine compound,
precipitating said layered double hydroxide having the fluorine compound between layers and the polymer containing fluorine,
recovering a solid part by a solid-liquid separation,
dissolving said recovered solid part in an acid, and
separating a fluorine compound or its salt.
[3] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to above mentioned process [1 ] or [2], the process further comprising,
adjusting pH of the solution to more than 4,
precipitating the layered double hydroxide having the fluorine compound between layers and the polymer containing fluorine compound.
[4] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to above-mentioned process [1] or [2], the process further comprising,
adding an alkali to the solution to adjust pH from 4 to 12,
adding divalent and trivalent metal salts to said solution, and
precipitating the layered double hydroxide having the fluorine compound between layers and the polymer containing fluorine.
[5] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to any one of above-mentioned processes [1] to [4],
wherein the divalent metal salt is a salt of magnesium, calcium, zinc, nickel, copper, manganese (divalent), or cobalt (divalent), and the trivalent metal salt is a salt of aluminum, iron, chromium, manganese (trivalent), cobalt (trivalent), potassium, lanthanum, or scandium.
[6] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to any one of above-mentioned processes [1] to [5],
wherein the divalent and the trivalent metal salts are chlorides.
[7] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to any one of above-mentioned processes [1] to [6],
wherein said fluorine compound is carboxylic acid or sulfonic acid having the fluorocarbon chain, in which the number of carbon is more than 5.
[8] The treatment process of the solution containing the fluorine compound and the polymer containing fluorine according to any one of above-mentioned processes [1] to [7],
wherein the polymer containing fluorine is poly-tetra-fluoro-ethylene.
[9] The treatm
Fuda Kiyoshi
Kamiya Takeshi Na
Matsunaga Toshiaki
Omori Kota
JEMCO Inc.
Richter Johann R.
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