JP2000509009A - Boehmite alumina salt - Google Patents

Abstract

  (57) [Summary] Cationic fibrous acetate salt of boehmite alumina useful for textile dyeing.

Description

DETAILED DESCRIPTION OF THE INVENTION                           Boehmite alumina salt   The present invention relates to a cationic fibrous acetate of boehmite alumina. Salt and its preparation and its use in dyeing fabrics such as cotton And waste removal from wastewater streams, for example dye-containing wastewater streams. is there.   Dyeing generally involves contacting a dye-containing solution with a fiber or a fabric of many fibers. , Thereby incorporating the dye into the lattice of entangled fibers or lattice It is carried out by adhering to. After that, the fiber or fabric is washed and Dyes that are not fully adhered or fully incorporated Remove the new dye. Until now, dyes that have not been incorporated or adhered are: The wastewater was discharged as wastewater together with the used dyebath, and the concentration was higher than that of the washing wastewater. This not only wastes considerable amounts of expensive dyes, but also drains the wastewater into rivers. It was necessary to purify it before discharging it. The dye (dye) used here The term is used to refer to dyes and pigments for carriers and for formulations or combinations, fillers, etc. Contains additives.   The present invention relates to a base suitable for use in dyeing and in purifying wastewater streams or wastewater. It relates to a salt of mitite alumina. The present invention also provides for aggregation and / or precipitation. And purification of urban wastewater streams and dye wastewater streams. When dyeing textiles, Useful materials in the dyeing process to remove significant amounts of dye from dye wastewater streams. Performance can be used to increase efficiency and reduce processing costs.   New cationic fibrous acetate salts of boehmite alumina (cake, chips, granules) Contacting the dye wastewater stream with other ionic species. It has been found that the dye aggregates or precipitates without contaminating the water stream. Therefore , Boehmite alumina salts are not only useful in the dyeing process, but also Is present as a pollutant in municipal wastewater streams or residual dye in dyebath wastewater streams Whether it is present (not incorporated or adhered to the fiber) Instead, the dye (e.g., anionic dye) may precipitate, bind, and / or aggregate. Can also be. Optionally, the removed dye can be recycled in the dyeing process Good.   Thus, in one aspect, the present invention provides a slurry of water and basic aluminum acetate. Stir, mix them substantially completely, react the slurry, -Potential greater than about 25 and aluminum to acetate weight ratio of greater than 4 By forming fibrous cationic acetate salts of small boehmite alumina Provide a obtainable cationic fibrous acetate salt of boehmite alumina .   One of the advantageous features is that the ratio of surface area to volume of the salt according to the invention is about 50% This is a good thing.   Conveniently, the active / reactive sites of the fibrous acetate are commercially available colloids. At least about 40% more than alumina.   In a further aspect, the present invention provides a cationic fiber of boehmite alumina according to the present invention. The present invention provides a method for preparing a fibrous acetate salt. The above-mentioned preparation method comprises the steps of: Stir the slurry of luminium acetate to mix them substantially completely, The slurry was allowed to react and the zeta potential was greater than about 25, Fibrous cation catalyst of boehmite alumina having a weight ratio to tate of less than about 4 It produces acetate salts.   Conveniently, the slurry comprises from about 0.5% to about 30% by weight of Al_TwoO_ThreeGood Preferably about 0.5% to about 15% by weight of Al_TwoO_ThreeTo (Al_TwoO_ThreeOn a basis). The slurry may be prepared for less than about 1 minute to about 60 minutes, preferably about 5 minutes, prior to initiating the reaction. Stir for about 30 minutes to about 30 minutes. The slurry is preferably at a temperature of about 100 ° C to about 180 ° C, Alternatively, the reaction is performed at about 140 ° C. to 160 ° C., and the reaction is performed for less than about 1 second to about 240 minutes. Desired The slurry is allowed to react for about 10 to about 120 minutes, depending on the type of end product. obtain. Conveniently, the slurry has about- The reaction can be performed at 140 ° C. for about 120 minutes. When manufacturing other types of products, Is reacted at a temperature of about 153 ° C. for less than about 5 seconds, in which case the temperature of the slurry When the temperature reaches 153 ° C., the temperature rise is stopped and cooling is started. The slurry is It is preferred to stir at a speed of about 50 to about 800 rpm during the reaction. After the reaction is over, Preferably, the slurry is cooled to a temperature from about 20 ° C to about 100 ° C.   The present invention further provides a dye selected from direct dyes, reactive dyes, sulfur dyes and acid dyes. And a fiber dyeing process using the same. In the fiber dyeing step, No fibers are converted to the cationic fibrous acetate salt of boehmite alumina according to the present invention. Through a reservoir containing bound or attached dye, thereby contacting said dye The fibers convert the dye from the fibrous acetate salt of boehmite alumina. Remove.   The present invention, in another aspect, provides a process for treating a dye wastewater stream. The processing step In the water stream, the cationic fibrous acetate of boehmite alumina according to the present invention is added. At least one coagulant or precipitant containing salt, the precipitate of the dye and the drug Alternatively, an aggregate is formed, and the precipitate or aggregate is separated from the water stream. The flocculant or the precipitant itself is also a further aspect of the present invention, and includes inorganic salts, coagulation Ingredients selected from agents, organic flocculants, polymeric flocculants, and mixtures thereof. May be contained.   The dyeing step and the dye removing step will be described with respect to the direct dye. , Those steps may involve other dyes, such as direct dyes, acid dyes, sulfur dyes or Equally suitable for reactive dyes, and any dyes having a negative or partially negative charge It should be understood that it can be used.   In the treatment step, the drug is advantageously converted to the dye contained in the dye wastewater stream. Have the opposite ionic charge, so that the dye is Adheres to The drug has a positive ionic charge and the dye has a negative ionic charge Is preferred. The step comprises adjusting the pH of the wastewater stream and the fibrous acetate suspension to about Preferably, adjusting comprises between 2 and about 8. The precipitate or aggregate Is conveniently removed by flotation and filtered. And the precipitate or Separating the dye from the agglomerate; and A step of regenerating the dye may be included. Such regeneration can be effected by the precipitation or Represents the aggregate, e.g. OH^-Or CO_Three ^-2By contacting the load You may. Optionally, the separated or regenerated dye is It may be used again in the color step.   A further aspect of the invention is a process for removing pollutants from a municipal waste treatment stream. is there. In the above step, the cationic fiber of boehmite alumina according to the present invention Adding a soluble acetate salt to the wastewater stream to form contaminants and salt precipitates or agglomerates; The precipitate or agglomerate is separated from the wastewater stream.   Prior to the present invention, dye wastewater streams were generally treated and discharged as wastewater. this By using the above process, the dye can be removed. Can be recycled, and the substantially dye-free water stream can be reused or discharged.   Advantageously, the fibrous acetate salt of boehmite alumina comprises the dye Has the opposite ionic charge. The fibrous acetate has a positive charge and the dye has a negative charge. It is preferable to have a charge. The dye is positively charged because it is negatively charged Attracts and adheres to fibrous acetate. Due to the difference in charge, the dye and the fiber The degree of reactivity or adhesion between fiber acetate is increased. Thoughts of the fiber of the present invention Some of the excellent results are due to the adsorption of the dye to the fibrous acetate surface. It depends. However, the charge difference between the fibrous acetate and the dye The apparent aspiration that the reactivity resulting from the removal of significant amounts of dyes from wastewater streams This is considered to be a major factor in unsuccessful results.   The pH of the wastewater stream is between about 2 to about 8 by adding an inorganic or organic acid. To promote precipitation or agglomeration of alumina acetate monohydrate salt fiber and dye Is preferred. The dye (excluding the reactive dye) is regenerated or separated, and the dyeing process is repeated. May be used. Particularly preferred is when the pH of the wastewater stream is between about 3 and about 5. Results are obtained. Prior to a sufficient amount of fibrous acetate in any convenient way It can be added to the dye wastewater stream.   One method of separating the sediment or aggregate is to use a floating separator. . The particles may be suspended by supersaturating them with air under pressure. So Thereafter, when the pressure is released, the air in the suspension lifts the particles to the surface. Soshi To remove suspended particles using a mechanical skimmer and discharge wastewater that has been bleached. You. Thereafter, the particles are circulated by any convenient means, May be used. By filtering through a filter, the concentration of the particles Can also be raised. Alumina monohydrate fiber used in the precipitation or aggregation step Many of the ratios can easily be returned to the original state. Flotation is preferred Although a separation method, the dye removed is known to those skilled in the art, such as high pressure filtration. Separation can also be achieved by other known methods. However, high pressure filtration is Requires more energy than floating separation.   An important aspect of the present invention is that, in certain instances, the dye can be regenerated and the dye It is possible to return to the process and reuse it. As mentioned above, fibrous acetate Solubility due to the difference in charge between the dye and the dye is a major factor in the unexpected results of the present invention. It is considered to be. The dye replaces the negatively charged group with a negatively charged dye, and the fiber It may be regenerated by releasing the dye from the acetic acetate. A convenient thing Indeed, such negatively charged groups are OH^-Or CO_Three ^-2And the like. The sediment Alternatively, the aggregates are filtered, using a negatively charged group, and mixed with alumina acetate monohydrate salt fiber. Contacting a filter cake containing a dye, replacing the negatively charged group with a dye, The material is preferably released and reused.   The process of removing dye from a dye-containing wastewater stream according to the present invention can be performed in batch or continuous. May be applied.   In industrial processes, textile dyeing can be an environmental hazard. For industrial processes, 90 Heat the dyebath to ℃ and use either chloride or sulfate for proper coloring It is necessary to add sodium salts up to 10%. Before dyeing the fabric, Heating the dye solution by applying fibrous alumina acetate (pre-treatment) The need to do so and the need to add salts can be reduced or eliminated.   The salts according to the invention may be prepared from basic aluminum acetate. Said Basic aluminum acetate may be prepared from alumina trihydrate and acetic acid . At high temperatures and pressures, basic aluminum acetate is hydrolyzed and A sum may be produced. Alumina monohydrate polymerizes to form fibers. general The process can be represented as follows.   The above equation shows the composition of boehmite. However, the product of the present invention is actually -Might acetate salt. Basic aluminum acetate is Al_TwoO (CH_ThreeCO_Two)_Four・ H_TwoIt can also be generalized as O. The sol product is alumina Consists of monohydrate fiber, acetic acid and water.   Reaction conditions, temperature, solids concentration, pH and stirring speed determine fiber dimensional characteristics . Fibers with new and unexpected dimensional property ranges are, for example, short and very It has been found to be produced in a wide or soft, hairy fiber. Solid concentration And temperature are parameters and are directly related to the fineness and dimensions of the fibers and bundles. Influence. Fiber bundles are large aggregates or aggregations of single fibers. And are produced under specific reaction conditions.Example   The highly cationic boehmite alumina acetate fibrous solution of the present invention has a pressure capacity Preferably, it is produced in a vessel (eg, a Parr reactor model 4522M). Sura It is possible to use any type of equipment that can quickly heat and cool the it can. The process can be conveniently summarized in the following four steps. (1)Preparation of BAA slurry:   1357 g of deionized water was converted into 143 g of in-house prepared basic aluminum acetate (B AA) and the slurry was stirred for 10 minutes. And prevent any settling The stirred slurry is quickly placed in a Parr reactor and stirred. The heating speed was set at 200-400 RPM and heated to high temperature. (2)Rapid heating to moderate temperature:   The heating rate was initially varied from 4 ° C / min to 5 ° C / min as the desired temperature was approached. Was. (3)Minimum reaction time at desired temperature:   Once the desired temperature has been reached, stop heating and allow the solution to have a reaction temperature for less than 1 minute. Ice water was immediately pumped into the cooling coil in the reactor to make it full. (4)Cooling and discharging:   Cold water was pumped through the cooling coil while stirring was continued. Contents reach 50 ° C The pumping was stopped and the solution was drained. The cooling process took about 10 minutes.   Complete the hydrolysis of BAA and control the growth of boehmite alumina acetate fiber Modest reaction temperature (140-160 ° C) is required with minimum reaction time . Small fibers provide the desired charge density as well as a higher specific surface area.   The alumina monohydrate sol product was dried at 350 ° C. Boehmite alumina The high cationic character of the acetate salt is due to its reaction / fixation with the textile dyeing staff, and It works to improve wastewater.   The characteristics of alumina acetate salt fibers can be determined by, for example, scanning electron microscopy (SE M), transmission electron microscopy (TEM); thermogravimetric method and acid titration of acetic acid content in sol Particle size analysis; and various well-known analytical techniques such as zeta potential. Further , Textile dye adsorption maximum, elemental analysis, thermogravimetric analysis (TGA), X-ray diffraction and infrared Light provides further information regarding the properties of the alumina sol.   In a 2-liter Parr reactor, 3.0 weight percent at 140 ° C for 2 hours. Al_TwoO_ThreeA sol was produced (Sol A). Under these reaction conditions, short and fine fibers A sol was produced. Hold at this temperature in the same reactor at 153 ° C Zeroing the time, for example, heating the mixture only to that temperature, 3. 0 weight percent secondary Al_TwoO_ThreeA sol was produced (Sol B). The latter substance is very It contained only small fibers (length <145 mn (TEM)). Sol A and B sump Air at ambient temperature and perform elemental analysis on aluminum, carbon and hydrogen. Was. Air-dried each sample using a DuPont 9900 thermogravimetric cell. In contrast, TGA was performed. In the first run, the temperature is raised to 650 ° C (20 minutes per minute). °) before drying the sample at 80 ° C for 15 minutes, in a second run the drying time Without providing, the temperature was raised to 650 ° C. Add an additional sample of air-dried sol to 8 Heated at 0 ° C. for 17 hours and another sample was heated at 350 ° C. for 2 hours. Similarly, two The air dried samples were tested by TGA experiments. For one, the temperature is 20 minutes per minute ° C and the other at 2 ° C per minute. X-ray diffraction was performed on these dried zones. Was carried out for Infrared spectra of the air dried sol were obtained.Elemental analysis 1.Sol A   Elemental analysis of the air-dried sample of Sol A showed C 4.92%, H 3.08% , And Al. 32.32%. The difference from this sum (40.32%) is considered to be 59.68 oxygen. available. If carbon binds only to acetate ions, The weight is calculated as 12.10% and is assigned as C 4.92%, H 0.62%, O 6.56%. Remaining The contents of H, O, and Al are determined by the moles of acetate and these components, and normalized. d) Shown below along with moles and charge balance.   Although the charge is not perfectly corresponding (+5.03 vs. -5.27), this is Probably due to slight errors. Two aluminum atoms in this material For example, assuming that it is alumina, the material The empirical formula (molecular weight 155.03 g / mol) is expressed as follows.                     Al_TwoO_2.83(CH_ThreeCOO)_0.34・ 2H_TwoO 2.Sol B   Elemental analysis of the air-dried sample showed C 8.79%, H 3.70% and Al 3 0.60%. The elemental analysis of that component (including 21.6% total acetate) gave C 8.79. %, H 1.10% and O 11.72%.   Thus, this sol contains significantly more acetate than Sol A. It The remaining percentages for these components, together with the calculated acetate, are given below. Write.  The charge equilibrium above relates to the analysis of this substance / compound, for example +5.28 vs. -5.32. Seems pretty good. The compound has two empirical formulas Assuming that it contains a nitrogen atom, the compound is shown below.                       Al_TwoO_2.68(CH_ThreeCOO)_0.64・ 2.25H_TwoODye adsorption   The dye adsorption of CI direct (dye) red 80 on the newly formed sol A_TwoO_Three The dye was 2800 mg per gram. However, "old" sol-containing sumps A value of approximately 5000 mg per gram of alumina is observed for the All ace If one adsorption site exists in the tate molecule, the number of sites is alumina Al_TwoO_ThreeGram It is calculated as 0.033 mol. 1417 g / mol molecule for direct (dye) red 80 Based on the amount, if one dye molecule per site is adsorbed, the theoretical adsorbable dye The charge is calculated to be 4700 mg per gram of alumina. Therefore, the empirical formula is Consistent with dye adsorption.   Similarly, for sol B, the calculated adsorption (one adsorption part per acetate ion) Alumina AL_TwoO_Three0.0062 mole of sorbent per gram You. For CI direct (dye) red 80, the expected adsorption is approximately It would have been around 8800 mg. This is not seen in newly generated sols. However, the "aged" sol of this material has about 8000 mg of adsorption per gram of alumina. Is shown.Thermal analysis   The thermal residual weight of sol A when heated to 650 ° C._TwoO_ThreeCompound On the other hand, it is calculated to be 65.66%. The measured residual weight is 69 if not initially dried. It was found to be .50% (FIG. 1). This is some loosely bound acetate May be lost as acetic acid at atmospheric conditions prior to thermal analysis. An example For example, only about half of the molecular weight of acetate actually binds to alumina and the rest Is simply absorbed by the solid as acetic acid,_TwoO_2.91(CH_ThreeCOO)_0.17 ・ 1.92H_TwoWhen O is heated, the theoretical residual weight is 70.27%. 1) Loss of loosely bound acetic acid and water: 2) Sample heated to 650 ° C:   This explanation is consistent with the direct (dye) red 80 adsorption. For example, the amount of dye adsorbed is Would be expected to be about 2400 mg per gram of alumina.   Additional samples were prepared by infrared spectroscopy and heat treatment to characterize . To determine the nature of the chemical components that will be lost at 80 ° C, Heated at C for 17 hours. The residual weight for this sample was determined to be 93.72% ( Figure 2). Similarly, if the sample was heated at 350 ° C for 2 hours, the residual weight was determined to be 77.60%. (Figure 3).   An air-dried sample of Sol B was tested thermogravimetrically. The sample was exposed The maximum temperature was 650 ° C. At that temperature, only alumina, as shown below, It is expected to remain.   The residual weight calculated based on this formula is 58.24%. See in Figures 4 and 5 Thus, for two temperature ramp rates of 20 degrees per minute and 2 degrees per minute, the residual weight is 6 It was found to be 1.59% and 61.99%.Infrared analysis   Infrared spectroscopy of air dried AMS material sample using potassium mul Obtained. Samples were 1) at room temperature, 2) 17 hours at 80 ° C (see Figure 6), and 3) 2 hours at 350 ° C. While drying. Approximately 1600 cm of ionized acetate salt^-1Clearly indicated in the above Providing further evidence that the AMS substance is indeed an acetate salt or compound I have. The spectroscopy of all samples is shown in FIG. 7, each of A) treated at 350 ° C. for 2 hours. B) treatment at 80 ° C. for 17 hours, and C) air drying at room temperature. Whole minute As seen in light, there is a chemical structure of the salt. 1) Handbook of Chemistry and Physics; Eee. R. (Lide, D.R.); Ed. -In-Chief (Ed.-in-Chief); 73rd edition (7 3rd ed.); CRC Press, 1993; 9-152. 2) The infrared Spectra of Minerals; Farmer , Vui. C. , Ed. (Farmer, V.C., Ed.); Mineralogical Societ y), 1974. 3) Maximov, Vui. N. (Maksimov, V.N.); Grigordev, A. Eye . Jay. In Auger. Chemi. Grigor ev, A.I.J. Inorg . Chem. USSR (English translation) 1964, 9 (4), 559-560. 4) Infrared Spectra of Inorganic Compounds Nyquist, Earl. A. (Nyquist, R.A.); Kargel, R .; Oh. , Ed. (Kagel, R.O., Ed); Academic Press, 1971. As can be seen from the TGA (FIG. 1), a significant weight loss (16.60%) occurs above 350 ° C. The weight loss measured above 350 ° C is calculated by the following empirical formula, Al_TwoO_2.91(CH_ThreeCOO)_0.17・ 0.08 5H_TwoO, the theoretical weight loss is calculated to be 13.24% and measured It is in good agreement with the fixed value. Therefore, only water is lost at these temperatures and alumina The acetate salt remains relatively intact.X-ray diffraction   X-ray diffraction of sol A air-dried at 25 ° C. showed a width consistent with boehmite alumina. A broad diagram was shown (FIG. 8). The broadening of the line is due to the alumina present in the sample. This is due to small particles. The main differences observed are, for example, d-spacin Approximately 6.635 angstroms versus boehmite, such as 6.110 Seen at the first peak at 14 degrees 2-theta. Of course, this is vinegar What would be expected if the acid were clearly bound to alumina fibers, for example, a salt complex. It is.   To further examine this peak at d = 6.635 A, confirm d-spacing So I did a second diffractogram. As shown in Figure 9, the same diffraction was obtained Was. However, when the sample was dried at 80 ° C, it was 6.6 Å. D-spacing moved to 6.375A (Figure 10), approaching that of boehmite . This suggests that this salt complex is thermally reacting at 80 ° C. Matches the result. The results of all these diffractions are summarized below.  For the dried sample of sol B, several other A small peak is observed. (See FIG. 11). Most important with boehmite alumina Reversal occurs at about 6.8 angstroms and the alumina acetate salt / complex Seems to be unique to.wrap up   Elemental analysis, thermal studies, infrared spectroscopy and X-ray diffraction indicate that sol solids Aluminum salt of high cation charge or acetate It supports the fact that it has a contrast. Sol A and air dried at ambient temperature The empirical formulas for B and B are consistent with dye adsorption studies, and thermogravimetric analysis and infrared spectroscopy Al_TwoO_2.83(CH_ThreeCOO)_0.34・ 2H_TwoO and Al_TwoO_2.68(CH_ThreeCOO)_0.64・ 2.25H_TwoBest suited for O ing.                                 Example 1   A slurry was made with water and basic aluminum acetate (BAA). The slur The amount of BAA used for Lee was Al_TwoO_ThreeChanges from about 1% to about 5% (w / w) based on I let it. Once the appropriate amount of water is added to make the total amount 1500 grams, The slurry was stirred for 10 minutes with a stirrer. This slurry to prevent any settling Quickly remove the two lids of Parr Reactor Model 4522M. The reactor was placed in a pressurized reactor. Set the heating rate high, and within 30-45 minutes, The device was at the desired temperature. Take a 2 to 5 gram sample at this point and Additional samples were taken every 30 minutes thereafter.   After reacting for 2 hours at the desired temperature, remove the reactor from the heating source and And cooled to about 70-80 ° C. Open the reactor and remove the birefringent alumina sol. And removed a sample for physical characterization. PH, viscosity, The percent of acetic acid was measured. By transmission electron microscope (TEM), the product sol Aliquots were characterized for fiber size.   Table 1 contains the reaction parameters for the experiments performed by the three factor study. . Table 1: Reaction parameters  From the TEM photograph, it was confirmed that three new fiber shapes were produced (see Table 2). ). The first are short, wide monofilaments, which were produced during cold runs Met. The second is a long, curvy, hairy fiber, obtained at 160 ° C. It is. The third was a fiber bundle, which looked like a large agglomerate of single fibers. Table 2: Single fiber size range and average value   Table 3 summarizes the dimensional data of the fiber bundle. Fiber bundles have specific properties It is a solidified fiber having. Sols containing fiber bundles have a high sedimentation rate. This Separation performance allows the fiber bundles to be highly sedimented to precipitate environmentally undesirable Can be used for applications where the rate is available.   Products reacted at 180 ° C are higher than those reacted at lower temperatures. Contains a proportion of fiber bundles. Fiber bundles can be up to 3.8 microns wide and long Varies from 18.2 microns. Table 3: Fiber bundle size average data  Table 4 contains the physical characterization data of the final product samples obtained. You. These data were recorded by computer for the pressure, temperature and temperature during the reaction. And stirring speed, which is extremely important for comparing the runs. Is shown Thus, the ratio of acetic acid, PH and viscosity are all_TwoO_ThreeDepends on the percentage of solids concentration ing. 1% Al in final product_TwoO_ThreeIn the sol, the proportion of acetic acid is about 2% However, 3% sol contains about 6.5% and 5% sol contains acetic acid. Was 11 percent. The percentage of acetic acid was determined by titration against caustic soda. Was. The pH of each sol also changed with concentration. Viscosity varied with concentration and temperature . The viscosity of the 1% sol was below the lower limit of detection of the viscometer. 5% sol is 16,100 cells It had a viscosity of up to nichipoise (cps). Table 4: Summary physical data of the final product  Analysis of these experimental data showed the following correlations: 1 ) Fiber length is increased by increasing reaction temperature; 2) Fiber width is lower 3) Fiber bundle length is longer at higher concentrations; 4) Sol viscosity The degree increases as the concentration increases and decreases as the temperature increases.                                 Example 2   Dilute the sol with deionized water until the alumina concentration is 0.75% w / w and mix thoroughly. Was. The fabric was weighed before and after treatment and the weight percent pick was increased. Tar Get pickups were 80 percent of the original pretreatment weight. The fabric , Dried in an oven at 50 ° C, then at ambient temperature 1 gram of dye / Staining in a solution containing the solution. After dyeing, put the fabric in the oven , Dried, with commercial control (90 ° C, 10 wt% NaCl) for strength and even coloration Compared visually.   When dyeing textiles with the sol produced in Example 1, certain sols are: It showed significantly better dye adsorption than the others. Prepared at 140 ° C for 2 hours, 3% Al_TwoO_Three And the sol containing short, fine fibers performed the most promising dye adsorption. these Textile samples are analyzed by reflection spectroscopy commonly used in the textile industry to The K / S value, which is an indicator of the shade of the color tone, was obtained (where K is the absorption coefficient, S Is the scattering coefficient. AATCC Evaluation Procedure 6 , 1996, see AATCC Technical Manual 1996). Short The K / S value obtained from the fabric treated and dyed with fine fibers (Examples 6 and 22) is 6.368. Was. The value of a commercial dyed product (e.g., 10% salt at 90 ° C.) that has undergone a mock test is: 5.346. Therefore, the addition of aluminum monohydrate sol allows the dyeing of textiles. The strength of the material has improved. The reflectance test procedure is based on standard (ASTM) procedures used in the textile industry. It is order. Using this test and interpolating the resulting data, Significantly strengthens fabrics so that additives are enough to be bought and sold in the market Can be determined.   The dye concentration in the supernatant is determined by using the obtained absorbance and a standard plot. Can be determined. The amount of dye adsorbed by the sol is the amount of dye at the start and remains in the supernatant Is the difference from the amount For example, the supernatant diluted by centrifugation If the dye is found to have a concentration of 0.040 mg per ram, this dye is The ability of this sol to adsorb can be calculated as follows.   Amount of excess dye: 0.040mg / g × 60 × 200g-480mg   Amount of dye adsorbed: 600mg-480mg = 120mg   Adsorption capacity: 120mg / 0.20g-600mg / g Where 0.040 mg / g is the dye concentration of the diluted supernatant obtained from the standard plot. , 60 is the dilution factor for the supernatant, 200 g is the total weight of the mixture, 600 mg Is the amount of dye at the start and 0.20 g is the amount of AlOOH solids used. The result of this example is that 600 mg of this dye can be adsorbed on 1 gram of AlOOH solids. You can do it. Table 5: Textile dyeing experiment Adsorption from used dye bath   The general procedure of a dye adsorption experiment usually involves the following six steps:   1) Define a standard Beer's law plot   2) Prepare a dye solution and hydrolyze the dye only if it is a reactive dye   3) Mix the sol with the dye solution   4) Separate dye-adsorbed particles from water   5) Measure the amount of excess dye   6) Calculate the amount of dye adsorbed to get the adsorption capacity.Preparation of standard plot   First determine the maximum absorbance of the dye solution at six known concentrations by UV-visible spectroscopy. Obtained using The value obtained and the corresponding concentration (per gram of total solution) A plot of absorbance versus concentration was made for each mg of dye. Experimental Pro The quality of the kit was checked, and an optimal line was created using a computer. This line Was used for excess dye determination.Preparation of a mixture of sol and dye solution   Generally, not only the total weight of the mixture, but also the dye, sol, 0.1% polyacrylic acid The amount of each component, including mid (PAA) and water, is measured before each experiment. Attach to container The order of addition is: dye, water, sol, and PAA. However, the dye is It must be completely dissolved before adding the sol. Reactive dye space In this case, a step of hydrolyzing the dye is required before adding the sol.Measurement of excess dye   About 50 ml of the mixture was centrifuged (or filtered) at maximum speed for 2.5 hours. And The supernatant was diluted 20-120 times (by weight) for UV-visible experiments. The diluent Used for the range of absorbance in the standard plot. Usually, it is 0.2 to 1.5.   Table 5 summarizes the cloth (cloth) dyeing experiments, where short and fine fibers It shows that excellent dye-adsorbing action is obtained. Experiment number 6 is the best The reflectance values are shown. Therefore, the best tie to use for this purpose The fibers of the loop are fine fibers.                                 Example 3   To evaluate the dye adsorption performance of the 27 sol products obtained from Example 1, A testing was performed. In that experiment, the same amount of dye had the same solids concentration And 27 sol solutions. And by the adsorption of fibrous acetate The resulting decrease in dye concentration was determined by the change in absorbance obtained with a UV-visible spectrometer. Judgment by conversion. In these tests, a 10 ml sol solution (0.75% Al_TwoO_Threeconcentration) Is mixed with 0.5 ml of a 1 g / L concentration of dye (C.I. direct (dye) red 80) in a 15 ml centrifuge tube. did. After centrifugation for 2 hours, Perkin-Elmer Lambda 2 UV visible spec Using a trometer (Perkin-Elmer Lamda 2 UV-Vis spectrophotometer), The supernatant was examined in detail. Table 6 shows the absorbance of the screening test.               Table 6: Absorption values of dye absorption test results(Note) n / a^*-Slight absorption indistinguishable from background   The data in Tables 5 and 6 show that smaller fibers can better adsorb dye (dough On the other hand, the resulting particles are easily removed from the water Is too small (precipitation rate is low). Therefore, a large proportion of large fibers The sol product with bunches was used for the initial adsorption capacity test reported in this example. I chose. This takes advantage of the fact that these fiber bundles settle quickly. You. This type of sol contains 3% Al_TwoO_ThreeAnd a relatively high reaction temperature (180 C) for a long time (5 hours or more).   Experiments were performed on various dyes to confirm the adsorption capacity of alumina acetate. I went. As a general experiment, 0.600 and 0.500 g of the dye were combined with 193.73 and 193.83 g of the dye. H_TwoEach was dissolved in O. 5.67 g of sol was added to each dye solution and the total weight of the mixture To 200.00 g, and the container was shaken to mix well. And a part of the mixture Was centrifuged for 2.5 hours. For reactive dyes, before adding the sol, a pH range of 1 A hydrolysis step at 140 ° F. for 45 minutes was performed at 0.5-11.0. The sol was used in the experiment of Example 1. No. 9 parameter was used, but with a 5-hour reaction time, large fiber bundles It was prepared to account for a large proportion.   Before adding to the dye solution, alumina acetate monohydrate salt sol is added for 10 minutes or less. Stir up to ensure uniformity. In general, 5.67 g of this sol was used, Equivalent to .20 g of alumina acetate monohydrate fiber. The following calculations were used.   Al_TwoO_ThreeTotal solids: 0.03 × 1500g = 45.00g   Al_TwoO_Three・ H_TwoO solid total amount: (120g / 102g) x 45g = 52.94g   Al_TwoO_Three・ H_TwoO solid%: (52.94g / 1500g) × 100% = 3.35%   Or: 5.67g × 0.0353 = 0.200g   Excess (unadsorbed) dye was measured using visible spectroscopy to confirm dye adsorption. A standard Beer's law plot (absorbance vs. dye concentration) is plotted with a dye solution of known concentration. Was prepared first. Produced by centrifuging a mixture of sol and dye solution The supernatant was diluted 20- to 60-fold. Excess dye concentration, standard plot prepared earlier By calculating from the UV-visible absorbance based on The amount of dye adsorbed was measured. The amount of dye adsorbed depends on the starting dye concentration. When it became relatively unaffected, its absorption capacity was reached.   The capacity tests and results for the five dyes are summarized in Table 7.                        Table 7: Amount of dye absorbed (mg)   Concentrations 1 and 2 have starting concentrations of 2.5 and 3 g / L, respectively.   One important issue is the ability to regenerate the sol product. alumina A second batch of acetate sol (Run 2) was prepared using the reaction parameters of Run 1. Was done. Table 8 shows the two sol products prepared using the same reaction parameters. Compare the results.             Table 8: Amount of dye absorbed in different alumina sols (mg)   As another example, to simulate a production environment, NaCl or Na_TwoSO_FourIt was used . Table 9 shows the results.          Table 9: Effect of salt on absorption capacity Example 4   This experiment was performed to determine at which pH value the dye was adsorbed best. The adsorption at values 3, 4 and 5 was tested.   A dye solution was prepared at a concentration of 100 mg / L. Its pH value depends on the concentration of concentrated HCl or charcoal. Sodium acid (Na_TwoCO_Three). The amount and type for that adjustment will depend on previous experiments. Determined by Alumina acetate sol fiber diluted 60 times and 0.1% PAA Was added and the sample was centrifuged. The resulting capacity is described in Example 2. It was exactly what I did.   The sol used in Examples 5, 6, 7, 8 and 9 was the same as Experiment No. 6 of Example 1. Prepared using one reaction parameter. Alumina acetate fiber in dye solution The sol was frequently diluted to facilitate dispersion of the fibers.                                   Table 10   This data shows that as the pH of the dye solution approaches 3, alumina acetate salt fibers It shows that the performance of the fiber to adsorb the dye is significantly improved.                                 Example 5   At different concentrations of sodium chloride (NaCl), alumina acetate monohydrate The ability of the sol fibers to adsorb the dye was assessed. The previous experiment showed that the pH was more acidic Shows that the adsorption occurs favorably. Therefore, the dye solution is concentrated hydrochloric acid (HCl) Was adjusted using. Some of the dyes precipitated salts with high concentrations of NaCl. therefore These dyes were tested at low concentrations.   Prepare a dye solution for each of the six dyes tested, and Final concentration was 100 mg / L. Each pH was adjusted with HCl. 60-fold diluted Addition of alumina acetate monohydrate sol fiber and 0.1% polyacrylamide (PAA) The solution was centrifuged and analyzed by visible spectroscopy to confirm adsorption. (Implementation See Example 2).                                   Table 11 Example 6   Different concentrations of sodium sulfate (Na_TwoSO_Four), Alumina acetate monohydrate The performance of the dyestuffs to adsorb the dye was evaluated. The previous experiment was performed when the pH was more acidic. It shows that adsorption occurs favorably. Therefore, the dye solution is concentrated HCl Was adjusted using. Some of the dyes have high concentrations of Na_TwoSO_FourTo precipitate the salt. Soy sauce These dyes were tested at low concentrations.   Prepare a dye solution for each of the six dyes tested, and Final concentration was 100 mg / L. Each pH was adjusted with HCl. 60-fold diluted Add alumina acetate monohydrate fiber and 0.1% PAA, centrifuge the solution, Analysis was performed by visible spectroscopy to confirm adsorption (as described in Example 2).                                   Table 12   The pH of each solution was measured after obtaining a sample for centrifugation. In these solutions The addition of HCl did not lower the pH of the solution to 3, but rather approached 4. It turned out that it was. Therefore, empirically, if the pH is lowered to 3, More favorable results will be obtained.Example 7   This example demonstrates the use of alumina dyes at the temperature of common jet dyeing sewage from a commercial dyer. The ability of the acetate monohydrate sol fiber to adsorb the dye was tested.   A control dye solution with a concentration of 3 g / L was prepared as usual at ambient temperature. Test dye solution , 65 ° C and 85 ° C and a concentration of 3 g / L. Water used for dye container and dye dilution Was heated. Then, the alumina acetate monohydrate sol fiber was heated to about 40 ° C. The solution and sol were mixed while hot and poured into tubes and centrifuged while hot. The volume of the dye solution was measured by UV-visible spectroscopy as described in Example 2.                                   Table 13 Example 8   Standard acrylic latex white liquid coating agent, alumina acetate monohydrate The proportion of the hydrate salt was increased and mixed. The choice of this sol was This is because it has the effect of reducing the gloss and yellowing observed in the glass. This zo Is very sticky, but it is an electric laboratory turbine type stirrer (electric labo ratory turbine type stirrer) to the liquid latex coating agent. Easy to mix.   Apply liquid latex on plate glass panel, 48 hours Let dry. Measure the gloss and expose the same panel to UV radiation for 48 hours Exposed. The following results were observed:   1. Addition of sol significantly reduced gloss.   2. Addition of 1 to 11 weight percent colorless sol reduces gloss and increases The gloss improved when the weight exceeded the limit.   3. From the micrograph of the coating surface, the addition of sol to reduce gloss The texture of the surface becomes rougher, and the surface texture exposed to UV light No difference is seen with the uncoated surface.   The sol is an excellent addition to latex coatings to adjust gloss Was an agent. The mechanism of this phenomenon is as follows.   1. Water resistant to disperse very hydrophilic and colorless sols easily depending on the amount of water present Added to the acrylic latex liquid coating.   2. When the liquid coating is applied to the substrate, water is applied to the substrate. And lost compatibility in the absence of water.   3. The alumina acetate monohydrate particles formed non-dispersed fine particles. The granules When measuring gloss, the surface may be slightly affected without affecting color and scattered light. Make it rough.   The addition of a pigment of the selected fineness (particle size) is a standard method of adjusting gloss. You. This sol is colorless and does not interact, as a convenient coating additive Has excellent applicability.Example 9   Alumina acetate monohydrate salt fiber produced according to Example 1 (Experiment No. 6) In comparison with commercially available polymer electrolytes, their utility in wastewater treatment was determined.   Using the same basic procedure, the alumina acetate monohydrate salt fiber Performed bench-scale tests comparing inorganic and organic cationic polyelectrolytes Was. First test the products currently in use and establish their usage and performance levels. Testified. After establishing the baseline, a series of tests are performed using the fibers and A dose range was established. At that time, the performance was similar to the product currently used. Previous Once the usage range for the fiber was established, a series of direct comparison tests were performed. A final test is then performed to determine the specific performance characteristics (sedimentation rate, floc size, sewage Color and turbidity).Iron ore tailing purification   Iron ore preparation starts with raw ore and uses a magnetic separation process to remove silica I do. The ore is first mined with a series of wet balls and a rod mill. Ground to 500 mesh and then passed over a series of magnets. The ferric oxide is magnetic Collected on stone and separated from silica. Reject from magnetic separator , Still contains some iron ore, which can be recovered in a high speed granulator . Heavy iron ore precipitates and light silica does not precipitate and flows out of the system.   The rejects exit the high-speed particle sizer and pass through a large Purified using DMAC. Solids in this tailing stream vary from 3% to 5% It is. These units create 100 +/- 20 turbidity units for reclaimed water quality I do. The feed rate of liquid poly DADMAC (20% active) depends on how many milling cycles 1.0 to 1.5 mg / l depending on whether the road is operating. At low occupancy rates, the fee is 1. Close to 0 mg / l. This is because the time available for precipitation is longer. High utilization rate Then, in order to maintain good reclaimed water quality, more substances are needed.   Calibrated cylinder settling tests were performed on poly DADMAC and alumina acetate. This was performed to determine the rate of precipitation of the monohydrate salt fiber. 5 gallon tailing The sample was collected and the polymer was added to the sample. After mixing this slurry Take 1 liter sample from 5 gallon sample, 1 liter scale With cylinder. When the slurry passes the mark on the 1,000 ml graduated container, The time was recorded. These batch purification tests are performed in the next field of the purifier did. The recorded turbidity was evaluated based on a direct comparison with known samples.   The following summarizes data collected using poly DADMAC and the fiber. It is. Needed for the fiber to produce results similar to poly DADMAC Amounts ranged from 400 to 500 mg / l.                         5 gallon batch purification test   Sample number Amount used Sedimentation rate per 1.75 inch seconds Clarity                    MG / LITER Free sedimentation Compact sedimentation                               800ML ~ 600ML 500ML ~ 300ML 1. Poly DADMAC 1.5 21 23 Good 2. Poly DADMAC 1.0 24 27 pretty good 3. Alumina     acetate     Monohydrate salt fiber 500.0 20 24 Good 4. Alumina    acetate    Monohydrate salt fiber 400.0 28 30 Very good 5. Alumina    acetate    Monohydrate salt fiber 500.0 22 25 Good 6. Poly DADMAC 1.3 23 27 Good 7. Poly DADMAC 1.0 25 30 Very good 8. Alumina    acetate    Monohydrate salt fiber 400.0 33 60 Very good 9. Alumina    acetate    Monohydrate salt fiber 500.0 27 33 Very good Ten. alumina     acetate     Monohydrate salt fiber 600.0 23 26 GoodWastewater treatment   Over the years, municipalities have been working in large quantities (30 to 30) to remove color from textile mill wastewater. 40 mg / l) of a polyamine. The polyamine (50% active) is a CPS product Quality.   Fiber compared to polyamine and polyaluminum chloride (70% and 83% basic) A conventional jar test was performed to measure the performance of the jar. The first color decision is dirty This was done by comparing the water sample with the others. In the final series, Color filters each sample three times, treats each sample at three different wavelengths, Using color measurement means including using a computer to calculate the final color Processed. Untreated colors range from 600 to 800, and secondary sewage colors range from 375 to 4 Between 25. The test results are summarized below.                               Wastewater treatment equipment                       1 liter batch purification test Sample number Used amount Sedimentation rate Sludge amount Clarity                   MG / LITER 500 ML mark 15 minutes later Visual instrument 1. Polyamine 20 150 seconds 200ml 400 NR 2. Polyamine 30 135 seconds 200ml 300 NR 3. Alumina    acetate    Monohydrate salt fiber 500 180 seconds 220ml 350 NR 4. Alumina    acetate    Monohydrate salt fiber 1000 240 seconds 240ml 300 NR 5. PAC 70% base     23% Al_TwoO_Three         50 180 seconds 200ml 450 NR 6. Polyamine & 15     PAC 70% base 20 180 seconds 200 ml 250 NR 7. Polyamine &     alumina     acetate     Monohydrate salt fiber 150 200 seconds 220ml 300 NR 8. Polyamine & 20     alumina     acetate     Monohydrate salt fiber 100 170 seconds 210ml 300 NR 9. Polyamine 20 135 seconds 200ml 400 395 Ten. Polyamine 30 125 seconds 200ml 300 389 11． Polyamine 20     PAC 70% base 20 190 seconds 210 ml 200 394 12． Polyamine & 15     alumina     acetate     Monohydrate salt fiber 150 180 seconds 220 ml 300 385 13. alumina     acetate     Monohydrate salt fiber 300 160 seconds 210 ml 400 419 14. alumina     acetate     Monohydrate salt fiber 600 180 seconds 220 ml 300 399   Alumina acetate monohydrate salt fiber is comparable to polyamine at 600mg / l Brought. Sludge volume is slightly higher and solids are slightly lower than polyamines Settles slowly. The fibers have large flocs similar to polyamines However, PACs have very fine flocs. The fiber is measurable Performance is better than PAC type products.   Best results are obtained with polyamine (15-20 mg / l) and alumina acetate fiber (100 150 mg / l). Do this several times. , With excellent results. This is because factories have toxic problems and polyamines It is important if it is the cause.Municipal drinking water treatment   Municipalities are required to purchase aluminum sulfate or polyaluminum chlorosulfate (PACS). Use one to purify river water. And aluminum sulfate depending on the water quality And switch to PACS. Aluminum sulfate is 17% Al_TwoO_ThreeAnd PACS is 10.5% Al_TwoO_ThreeIs a 50% basic product. Low alkalinity, turbid If the degree is high, PACS is used. High alkalinity, high chromaticity in water In that case, aluminum sulfate is used.   All tests were performed in a constant temperature bath. 0.17 units of untreated river water It had turbidity. The following is a summary of the results obtained. "Flock type `` Floc Formation '' means that you can see very small flocs Seconds. "Flock size" is a small flock as "12" This is a relative number that becomes as large as possible. "Clarity" refers to distilled water for "1" and untreated water for "12" Is the relative clarity of water.                         1 liter batch purification test Sample number Amount used Floc Floc Clarity Turbidity pH               MG / LITER formation size unfiltered filtration 1. Al sulfate    Minium 30 180 seconds 7 3 14.7 5.1 6.7 2. Al sulfate    Minium 40 120 seconds 7 2 16.4 1.7 6.6 3. Al sulfate    Minium 50 60 seconds 8 1 2.2 0.2 6.5 4. PACS 30 120 seconds 6 2 14.1 2.0 6.7 5. PACS 45 80 seconds 5 2 1.6 0.3 6.7 6. PACS 60 45 seconds 4 1 0.6 0.1 6.6 7. Alumina    acetate    Monohydrate    Salt fiber 100 150 seconds 7 5 7.5 5.0 7.0 8. Alumina    acetate    Monohydrate    Salt fiber 150 60 seconds 5 4 6.0 4.0 7.0 9. Alumina    acetate    Monohydrate    Salt fiber 200 150 seconds 7 3 5.0 1.5 6.8 Ten. alumina     acetate     Monohydrate     Salt fiber 300 180 seconds 9 2 4.2 1.0 6.7 11． alumina     acetate     Monohydrate     Salt fiber 600 240 seconds 12 1 1.8 0.5 6.2 12． alumina     acetate     Monohydrate     Salt fiber 900 240 seconds 12 1 2.4 0.1 5.2   The following are required for good agglomeration (DS ONE), color and turbidity removal (DS TWO) for each application. It is a summary of fiber content.   Alumina acetate monohydrate salt fiber worked in all three applications. that is, From inorganic products (aluminum sulfate, PAC and polyaluminum chlorosulfate) Also acted similarly to organic polyelectrolytes (polyDADMAC and polyamines). The fiber is It has excellent floc forming properties and forms good floc with low usage. Larger amounts are required for color and turbidity removal.

[Procedure for Amendment] Article 184-8, Paragraph 1 of the Patent Act [Date of Submission] June 29, 1998 (1998.6.29) [Contents of Amendment] In the translated text attached to the document, “contains.” On page 1, line 26, “according to ...” on page 2, line 21 is corrected as follows. Thus, salts of boehmite alumina are not only useful in the dyeing process, but also where the dye is present as a contaminant in the municipal wastewater stream or the residual dye in the dyebath wastewater stream (not incorporated into the fibers or The dye (e.g., an anionic dye), whether present as non-attached), can also precipitate, bind, and / or aggregate. Optionally, the removed dye may be recycled in the dyeing process. Therefore, in one embodiment, the present invention reacts alumina trihydrate with acetic acid to produce basic aluminum acetate, releases the basic aluminum acetate, stirs a slurry of water and the basic aluminum acetate, They are obtained by substantially mixing them thoroughly and reacting the slurry to form a fibrous cationic acetate salt of boehmite alumina having a zeta potential greater than about 25 and a weight ratio of aluminum to acetate of less than about 4. And a cationic fibrous acetate salt of boehmite alumina. One of the advantageous features is that the ratio of surface area to volume of the salt according to the invention can be about 50% or more. Conveniently, the fibrous acetate has at least about 40% more active / reactive sites than commercially available colloidal alumina. In a further aspect, the present invention provides a method for preparing the cationic fibrous acetate salt of boehmite alumina according to the present invention. In the preparation method, alumina trihydrate is reacted with acetic acid to produce basic aluminum acetate, the basic aluminum acetate is released, and a slurry of water and the basic aluminum acetate is stirred to substantially convert them. Thoroughly mixed and then reacting the slurry to produce a fibrous cationic acetate salt of boehmite alumina having a zeta potential greater than about 25 and a weight ratio of aluminum to acetate of less than about 4. Advantageously, the slurry comprises about 0.5% to about 30% by weight of Al ₂ O ₃ , preferably about 0.5% to about 15% by weight of Al ₂ O ₃ (based on Al ₂ O ₃ )contains. -The claims of the translation attached to the document pursuant to the provisions of Article 184-5, Paragraph 1 of the Patent Act are amended as follows. Claims 1. Reacting alumina trihydrate with acetic acid to produce basic aluminum acetate, releasing the basic aluminum acetate, stirring the slurry of water and the basic aluminum acetate, mixing them substantially completely, And reacting the slurry to produce a fibrous cation acetate salt of boehmite alumina having a zeta potential greater than about 25 and a weight ratio of aluminum to acetate of less than about 4, which is a cationic fibrous acetate salt of boehmite alumina. . 2. The salt of claim 1, wherein the active / reactive sites are at least about 40% higher than commercially available colloidal alumina. 3. The salt according to claim 1 or 2, wherein the fibers are at least partially in the form of a fiber bundle. 4. The salt according to any of the preceding claims, wherein the slurry is reacted at a temperature from about 100 ° to about 180 ° C. 5. The salt according to any of the preceding claims, wherein the slurry is reacted at a temperature from about 140C to about 160C. 6. The salt according to any of the preceding claims, wherein the slurry is reacted at a temperature of about 140C. 7. The salt according to any one of claims 1 to 4, wherein the slurry is reacted at a temperature of about 180 ° C. 8. 7. The salt of claim 6, wherein the slurry is allowed to react for about 2 hours. 9. The salt of claim 7, wherein the slurry is allowed to react for about 5 hours. 10. Reacting alumina trihydrate with acetic acid to produce basic aluminum acetate, releasing the basic aluminum acetate, stirring the slurry of water and the basic aluminum acetate, mixing them substantially completely, And reacting the slurry to produce a fibrous cation acetate salt of boehmite alumina having a zeta potential greater than about 25 and a weight ratio of aluminum to acetate of less than about 4, which is a cationic fibrous acetate salt of boehmite alumina. Preparation method. 11. The undyed fibers are passed through a dye-containing bath bound or attached to the cationic fibrous acetate salt of boehmite alumina according to any of claims 1 to 9, thereby bringing the fibers into contact with the dye. A method for dyeing fibers using a dye selected from direct, reactive, sulfurized and acid dyes, whereby the dye is removed from the fibrous acetate salt of boehmite alumina. 12. A flocculant or a precipitant comprising the cationic fibrous acetate salt of boehmite alumina according to any one of claims 1 to 9, optionally selected from inorganic salts, a coagulant, an organic flocculant, and a polymeric flocculant. A flocculant or precipitant comprising one or more components. 13. The dye wastewater stream is charged with at least one flocculant or precipitant comprising the cationic fibrous acetate salt of boehmite alumina according to any of claims 1 to 9, forming a precipitate or agglomerate of the dye and the drug, A method for treating a dye wastewater stream that separates the precipitate or agglomerate from the stream. 14． 14. The method of claim 13, wherein the agent has an opposite ionic charge in the wastewater stream as the dye. 15. 15. A method according to any of claims 13 or 14, wherein the agent has a positive ionic charge and the dye has a negative ionic charge. 16. 16. The method of any of claims 13 to 15, comprising adjusting the pH of the wastewater stream between about 2 to about 8. 17． 17. The method according to any of claims 13 to 16, comprising adjusting the pH of the wastewater stream to about 3. 18. 18. The method according to any of claims 13 to 17, comprising separating and regenerating the dye from the precipitate or agglomerate. 19. The cationic fibrous acetate salt of boehmite alumina according to any of claims 1 to 9 is added to a wastewater stream to form a precipitate or agglomerate of contaminants and salts, and the precipitate or agglomerate is removed from the wastewater stream. A method of removing pollutants from a separated municipal wastewater treatment stream. 20. 20. The method of claim 19, comprising adjusting the pH of the wastewater stream to between about 2 and about 8. 21. A flocculant for use in treating waste containing the salt according to any one of claims 1 to 9 together with a polyamine.

────────────────────────────────────────────────── ─── Continuation of front page    (81) Designated countries EP (AT, BE, CH, DE, DK, ES, FI, FR, GB, GR, IE, IT, L U, MC, NL, PT, SE), OA (BF, BJ, CF) , CG, CI, CM, GA, GN, ML, MR, NE, SN, TD, TG), AP (GH, KE, LS, MW, S D, SZ, UG), EA (AM, AZ, BY, KG, KZ , MD, RU, TJ, TM), AL, AM, AT, AU , AZ, BA, BB, BG, BR, BY, CA, CH, CN, CU, CZ, DE, DK, EE, ES, FI, G B, GE, GH, HU, IL, IS, JP, KE, KG , KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MD, MG, MK, MN, MW, MX, N O, NZ, PL, PT, RO, RU, SD, SE, SG , SI, SK, TJ, TM, TR, TT, UA, UG, UZ, VN, YU (72) Inventor Paysec, Eugene             United States, 30215 Josiah,             Fayetteville, Maple Place             115

Claims (1)

[Claims] 1. Stir the slurry of water and basic aluminum acetate and substantially mix them Mix thoroughly and allow the slurry to react, the zeta potential is greater than about 25, and the aluminum Boehmite alumina fibers with a weight ratio of aluminum to acetate less than about 4 Boehmite al which can be obtained by forming a neutral cationic acetate salt Mina's cationic fibrous acetate salt. 2. Active / reactive sites are at least about 40% higher than commercially available colloidal alumina. The salt according to claim 1. 3. The fiber according to claim 1 or 2, wherein the fiber is at least partially in the form of a fiber bundle. Salt. 4. The method of any of the preceding claims, wherein the slurry is reacted at a temperature of about 100 ° C to about 180 ° C. The salt according to the above. 5. Any of the preceding claims wherein the slurry is reacted at a temperature of about 140C to about 160C. The salt according to the above. 6. The method according to any of the preceding claims, wherein the slurry is reacted at a temperature of about 140 ° C. salt. 7. The method according to claim 1, wherein the slurry is reacted at a temperature of about 180 ° C. Salt. 8. 7. The salt of claim 6, wherein the slurry is allowed to react for about 2 hours. 9. The salt of claim 7, wherein the slurry is allowed to react for about 5 hours. 10. Stir the slurry of water and basic aluminum acetate and allow them to substantially And the slurry is allowed to react, the zeta potential is greater than about 25, Boehmite alumina fiber with a weight ratio of minium to acetate less than about 4 Boehmite Door Obtainable by Producing Ionic Cationic Acetate Salt A method for preparing a cationic fibrous acetate salt of lumina. 11. An undyed fiber, the boehmite door according to any one of claims 1 to 9. Through a dye-containing bath bound or attached to the cationic fibrous acetate salt of Lumina And, by contacting the fiber with the dye, the fibrous property of boehmite alumina Removes the dye from the acetate salt, selected from direct, reactive, sulfurized and acid dyes A method for dyeing fibers using a dye. 12. The cationic fibrous alumina of boehmite alumina according to any one of claims 1 to 9. Flocculant or precipitant containing acetate salts, optionally inorganic salts, coagulation Agent, one or more components selected from organic coagulants, and polymeric coagulants Or a precipitant. 13. The boehmite alumina according to any one of claims 1 to 9 in a dye wastewater stream. Put at least one flocculant or precipitant containing thione fibrous acetate salt, dye and Forming a precipitate or aggregate of the drug, separating the precipitate or aggregate from the water stream; How to treat the separating dye wastewater stream. 14． Wherein the agent has an opposite ionic charge to the dye in the wastewater stream. 14. The method according to 13. 15. Wherein the drug has a positive ionic charge and the dye has a negative ionic charge. Item 15. The method according to any one of Items 13 and 14. 16. 14. Adjusting the pH of the wastewater stream to between about 2 and about 8. 16. The method according to any one of items 1 to 15. 17． 17. The method of claim 13, including adjusting the pH of the wastewater stream to about 3. The method according to any of the above. 18. Separating the dye from the precipitate or agglomerate and regenerating the dye. 18. The method according to any one of claims 13 to 17. 19. The cationic fibrous alumina of boehmite alumina according to any one of claims 1 to 9. Adding acetate salt to the wastewater stream to form a precipitate or agglomerate of contaminants and salts, Removal of pollutants from municipal wastewater treatment streams that separate sediments or agglomerates from wastewater streams how to. 20. 20. Adjusting the pH of the wastewater stream to between about 2 and about 8. The method described in. 21. Waste treatment comprising a salt according to any of claims 1 to 9 together with a polyamine. Coagulant used for