KR20120073608A - Multipurpose absorbent made from dwts and its manufacturing method - Google Patents

Abstract

PURPOSE: A multi-functional absorbent and a method for manufacturing the same are provided to simultaneously absorb basic odor and acidic odor and to control volatile organic compounds. CONSTITUTION: A method for manufacturing multi-functional absorbent includes the following: water purification sludge is stirred and pulverized; 5 to 15 parts by weight of a material selected from regenerated phosphoric acid and phosphoric acid is reacted with the pulverized sludge; the resultant product is aged in an aging bath for 6 to 12 hours; the aged product is introduced into a disc drier of 100 to 200 degrees Celsius; an absorbent is manufactured, and the moisture content of the absorbent is in a range between 20 and 40%; the absorbent is mixed with a liquid resin or a liquid latex, and the mixture is granulated by using an extruder heated to a temperature between 200 and 300 degrees Celsius.

Description

Multipurpose absorbent made from by-products from water purification facilities and its manufacturing method {Multipurpose absorbent made from DWTS and its manufacturing method.}

    The present invention exhibits excellent physicochemical adsorption capacity and effectively absorbs basic odors such as ammonia and trimethylamine, as well as acidic odors such as hydrogen sulfide and methyl mercaptan, and controls the VOC (volatile organic compounds). It is about.

Activated charcoal must be impregnated with basic substances when adsorbing acidic odors.The problem of limited efficacy that can be adsorbed, the problem of ignition, the highly volatile VOC (molecular weight 40 or less) is poorly adsorbed Greater than 150) is a problem that is not easily removable. In addition, in order to avoid excessive heat accumulation in the adsorption column, the activated carbon adsorption tower has been used as an adsorbent in various fields even though there are various problems such as the concentration should not exceed 10,000 ppm. This is because there is a shortage of adsorbents that offer the right price and ease of use as activated carbon.

A patent on the preparation of adsorbents using purified sludge is given in 0702602. The patent consists of mixing 100 parts by weight of water with phosphoric acid in the manufacturing process and maintaining a temperature of 100 ~ 120 ℃ in the stirring process, after the cooling process to make a deodorant through a drying process.

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Activated carbon, which has been used as an adsorbent, has been on a steady increase since 2005, according to 2005-2009 activated carbon import statistics (data from the Korea Customs Service). This may be due to the continuous intensification of air-related regulations and the increase in odor complaints due to the improvement of quality of life. On the other hand, activated carbon must be impregnated with basic substances when adsorbing acidic odors. Limited efficacy that can be adsorbed. If the boiling point is larger than 150), there is a problem that the desorption is difficult. In addition, in order to avoid excessive heat accumulation in the adsorption column, the activated carbon adsorption tower has been used as an adsorbent in various fields even though there are various problems such as the concentration should not exceed 10,000 ppm. This is because there is a shortage of adsorbents that offer the right price and ease of use as activated carbon. Recently, the use of adsorbents using porous materials such as zeolite and mesoporous is increasing, but it has its own problems, such as having to go through a separate processing process to reduce expensive price and hydrophilicity. In addition, the decisive problem is that activated carbon, zeolite and mesoporous are mostly imported.

The present invention seeks to provide a multi-purpose adsorbent that overcomes the limitations of activated carbon used as an adsorbent for adsorbing gaseous substances and exhibits better performance. More specifically, the present invention is to provide an adsorbent which is capable of adsorbing basic odors and acidic odors at the same time and controlling low molecular weight, high molecular toxic substances, and highly volatile noxious gaseous substances while removing flammability.

Method for producing an adsorbent according to the present invention,

A first step of stirring and crushing the purified sludge;

A second step of mixing and stirring 5 to 15 parts by weight of a material selected from the group consisting of regenerated phosphoric acid and phosphoric acid (or regenerated sulfuric acid and sulfuric acid) and crushed purified water sludge;

A third step of aging the second step reactant into a aging tank for 6 to 12 hours while operating the aging tank at regular intervals;

A fourth step of producing a granule-type adsorbent by adding the aged product of the third step to a disk dryer and rotating it while heating to 100 to 200 to adjust the water content to 20 to 40%;

A fifth step of granulating the liquid resin with the liquid latex corresponding to 10 to 20% based on 100 parts by weight of the adsorbent through the fourth step and granulating it with an extruder (extruder) heated to 200 to 300;

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In addition, when the step-specific features of the present invention are described in detail, the aging step of the third step is a necessary step to overcome the problems caused by the difference in water purification sludge properties according to the intake source and the difference between the rainwater and the influent components of the dry season. For this purpose, the quality of the adsorbent produced can be kept constant by aging into a aging tank designed separately. In the fourth step, it is important to use a disk type dryer because other types of dryers are not easy to control the particle size and are expensive to dry. For this reason, disc type dryers are necessary to maximize the usability and performance of the final product.

The present invention is expected to be effective in various fields.

First, the quality of life at home is the effect. The adsorbent of the present invention will contribute to improving the quality of human life by effectively controlling bad smells generated in shoe racks, bad smells generated in old refrigerators, bad smells generated in automobiles, bad smells coming from sewers, and bad smells generated from food waste. .

Second, there is an increase in farm competitiveness. Pigs have a mortality rate of 10 to 15%, and 2.3 million pigs die each year, which translates into W700bn. Considering that about half of all deaths from respiratory diseases occur, economic losses of about 350 billion won occur every year. The adsorbent of the present invention will effectively control the odor generated from pigs to improve the air quality in pigs, thereby improving the growth environment, improving the working environment, increasing the growth rate, and reducing the mortality, thereby contributing to the increase of farmers' income and competitiveness. will be. In addition, by controlling the odor generated from the poultry to contribute to the production of expensive fertilizer, the poultry can be used as a farming material. This effect will ultimately contribute to providing farming competitiveness.

Third is the export and import substitution effect. According to the Korea Customs Service statistics, imports of 32,000 tons in 2005 and imports of 40 billion won increased from 36,000 tons in 2009 to 80 billion won. This means that import prices are gradually increasing. On the other hand, activated carbon has various problems such as ignitability, deterioration of adsorption capacity for high concentration odor, inability to adsorb volatile odor, selective adsorption. However, the adsorbent of the present invention can supply a cheaper and more stable product because there are more adsorption target material than activated carbon. For this reason, it is possible to export overseas and replace the import of activated carbon.

Lastly, it is a virtuous cycle of resources and green growth. Domestic purified sludge is about 660,000 tons per year, of which more than 60% is buried in the ground in the form of landfills or landfills (virtually landfills). However, as is clear from the present invention or the cited invention, purified sludge is a valuable resource that can create high added value. It is the provision of valuable technology and products that can be interpreted to mean securing new oil fields or mines in an age where resources are important enough to secure resources. Therefore, the present invention will be referred to as a technology and a product that contributes to the virtuous cycle of resources and the government's efforts to achieve low carbon green growth through this process.

The representative diagram presented is a process drawing showing the granulation process according to the use of the product by mixing, reacting, ripening and drying the purified sludge and additives.

Hereinafter, the present invention will be described in more detail.

The adsorbent according to the present invention relates to a method of making an adsorbent using by-products generated in a water purification plant. Patents for making an adsorbent using purified sludge are disclosed in 0702602, but the patent is a purified sludge in a manufacturing process. Along with phosphoric acid in 1. mixed with 100 parts by weight of water and in the stirring process 2. to maintain the 100 ~ 120 3. through the cooling process is the difference from the present application technology. 1 to 3 processes described above have various negative factors such as increased manufacturing costs, increased production process complexity, increased initial investment costs, difficulty in process management, and increased post-treatment facilities. The applied technology can simplify the complexity of such a process, thereby reducing the manufacturing cost, reducing the initial investment cost, and increasing the convenience of quality maintenance by simplifying the process.

Looking at the applied technology in more detail,

A first step of stirring and crushing the purified sludge;

A second step of mixing and stirring 5 to 15 parts by weight of a material selected from the group consisting of regenerated phosphoric acid and phosphoric acid (or regenerated sulfuric acid and sulfuric acid) and crushed purified water sludge;

A third step of aging the second step reactant into a aging tank for 6 to 12 hours while operating the aging tank at regular intervals;

A fourth step of producing a granule-type adsorbent by adding the aged product of the third step to a disk dryer and rotating it while heating to 100 to 200 ° C. to adjust the moisture content to 20 to 40%;

A fifth step of granulating the liquid resin with the liquid latex corresponding to 10 to 20% based on 100 parts by weight of the adsorbent through the fourth step and granulating the mixture with an extruder (extruder) heated to 200 to 300 ° C;

And the like.

Looking at the features and composition principle of each step,

The first stage consists of a process that allows the reaction with additives to occur by releasing the dense state in the process of transferring the purified sludge to the manufacturing facility.

The second step consists of mixing and reacting by adding 5 to 15 parts by weight of a material selected from the group consisting of regenerated phosphoric acid and phosphoric acid (to regenerated sulfuric acid, sulfuric acid) to 100 parts by weight of purified water sludge. The applied technology reduces the production cost by using phosphoric acid recycled from waste generated as a by-product from the semiconductor process. In addition, sulfuric acid, which can be used alone or in combination, has the advantages of being 1/10 of the price of phosphoric acid, increasing the hardness of the produced product, and effectively controlling the properties of the purified sludge through strong dehydration. On the other hand, there is no significant difference in the quality of the product, which is more than a substitute for phosphoric acid.

The third step is a step of aging for 6 to 12 hours in a aging tank of the additives and the finished reactant after the reaction.

Purified sludge is divided into general appeals and streams according to the intake source, and there are differences in the characteristics of dry season and storm season depending on seasonal factors.

In addition, some water purification plants in Busan, where water purification sludge, which is generally classified as an inorganic sludge, as a source of water in the Nakdong River, are classified as organic sludges. Considering these differences, the aging process is the key process to make the product produce adsorbents that meet certain standards. The maturation tank has a cylindrical structure, an opening and closing hole for maintaining the air pressure, a control valve for adjusting the air pressure, and an impeller installed therein, so that the reactants undergoing the second step are exothermic due to chemical reactions in the aging process. When cushioning occurs, the process consists of adjusting the speed and conditions appropriately, and making sure that the physicochemical composition of the maturation meets the criteria given in Table 1.

Adsorbent Component Reference Table Compound Concentration Unit Al 19 to 24 % Fe below 10 % S 35 to 45 % Si 8 to 13 % Cl 10 to 15 % Other Ingredients 5 or less %

The fourth step consists in producing a granule-type adsorbent while adjusting the moisture content to 20 to 40% by rotating the aged product of the third step into a disk dryer and rotating while heating to 100 ~ 200 ℃. Aged product is put into the disc dryer through the transfer line in the GEL state and rotates while repeatedly contacting the disc, the disc rotating shaft maintaining the temperature of 100 ~ 200 ℃, the inner wall of the disc dryer, and goes through the drying process. Finally, it produces granule type adsorbent with water content of 20 to 40%. The granule type plays a role of gradually exerting the adsorption performance by preventing scattering and maintaining natural hardness for a certain time when using the product. If the water content of the adsorbent is kept below 20%, the water content of the binder becomes insufficient and becomes powdery. If the water content exceeds 40%, the water content is 20-40% because the high water content negatively affects the adsorption capacity. It is important to stay within.

The final step is granulation with an extruder (extruder) heated to 200 ~ 300 ℃ by mixing with 10-20% liquid resin to liquid latex compared to 100 parts by weight of the adsorbent made in the fourth step, Since the adsorbents require a certain shape and hardness above a certain level, the products used for gas phase (gas phase) removal or water treatment need to undergo granulation (assembly) .In this case, the binder is a liquid resin and a liquid latex. The compounding ratio of 10 to 20 parts by weight is suitable for 100 parts by weight of the adsorbent. When the amount of the binder is less than 10 parts by weight, it is difficult to maintain the hardness, and when the amount of the binder exceeds 20%, it is important to maintain the adsorptive capacity.

Hereinafter, specific embodiment of this invention is described. However, it should be noted that the following embodiments merely introduce one aspect of the present invention, and the present invention is not limited only to the embodiments shown in these Examples.

Example  1 ~ Example  3

100 kg of purified sludge was crushed using a crusher. Subsequently, the crushed purified water sludge was mixed with 85% regenerated phosphoric acid or 65% regenerated sulfuric acid, and the reaction process was continued for 2 to 3 hours, and then dried in a disk dryer for 10 hours to produce granule-type adsorbent. . Further, 50 kg of the adsorbent produced in Example 1 was mixed with 20 parts by weight of the liquid resin and the liquid latex with respect to 100 parts by weight of the adsorbent and extruded while heating the barrel of the extruder (extrusion molding machine) to 200 to obtain a pellet-type granular adsorbent. Produced. Details of the input amount of the purified water sludge, the recycled phosphoric acid and the recycled sulfuric acid, the preparation method and the granulation process are shown in Table 2 below.

Water purification sludge Regenerative phosphoric acid Renewable sulfuric acid Manufacturing method product Example 1 100 kg 15 kg 100 kg of purified sludge was crushed using a crusher. Subsequently, the crushed purified sludge was mixed with regenerated phosphoric acid having a concentration of 85%, and the reaction process was continued for 2 hours, and then dried in a disk dryer for 10 hours to produce granule-type adsorbent.

Example 2 100 kg 7 kg 100 kg of purified sludge was crushed using a crusher. Subsequently, the crushed purified sludge was mixed with regenerated sulfuric acid having a concentration of 65%, and the reaction process was continued for 3 hours, and then dried in a disk dryer for 10 hours to produce granule type adsorbent.

Example 3 50 kg of the adsorbent prepared in Example 1, a liquid resin, and 5 kg of liquid latex are mixed to extruder the barrel of the extruder while heating to 200 ℃ to produce a pellet-type granular adsorbent.

Test Example

In order to evaluate the performance of the adsorbent made by the application technology, various experiments were conducted to confirm the effect. We present the official test results applying the deodorant certification standard (EL.608) and KS I 2218 (2009) among the environmental mark based on the deodorization ability and environmental technology development and support for complex odors generated in pigs. .

1.1. Deodorization  Experiment-Donsa

1.1.1. Experiment period: September 3, 2010 ~ September 24, 2010 (18 days)

1.1.2. Deodorization Target: Piglets (area 264m ² )

1.1.3. Adsorbent: X-DEO (8kg)

1.1.4. Odor Measuring Equipment: 'Oder catch Hand-held type (Series: SLC-OH010 System)'-This equipment shows the value of 30 ~ 40 without odor.

1.1.5. Experiment Donsa: 70-2, Seong-ri, Cathedral-myeon, Iksan-si, Jeonbuk, Korea

1.1.6. Experimental conditions: The experiment was conducted to find out the removal efficiency of the gas due to the severe gas generation during the scraping process to remove the manure accumulated in the piglets. Intentionally keep the manure in the piglets upside down for the duration of the experiment.

1.1.7. Experimental method: After making the measurement standard in the fresh air state, the compound odor meter was measured at 3 days intervals by measuring the odor intensity with the compound odor meter at the middle point of piglets.

1.1.8. Experimental results: As shown in the graph below, it was confirmed that the odor concentration was significantly decreased after 6 days. In addition, it was confirmed that the adsorbent (X-DEO) made by the application technology controls the odor for a considerable period of time. In general, odors generated from pigs are a problem that a variety of odor sources such as ammonia, hydrogen sulfide, fatty acids, acetic acid, etc. act in combination to control only specific odorous substances, making it difficult to use as a housing environment improver. The adsorbents based on the applied technology have been evaluated as having excellent gas removal capability compared to the existing product ranges in the experimental farms. Below is a chart of the experimental results.

Odor control result table by period (combination of odor measuring instrument and sensory method) Measurement date Measurement period Measure Result by sensory method 10/09/03 Day 0 177 Extreme odor (4) 10/09/06 3 days 127 Extreme odor (4) 10/09/09 6 days 84 Strong odor (3) 10/09/12 Day 9 63 Normal odor (2) 10/09/15 Day 12 62 Detection odor (1) 10/09/18 Day 15 58 Odorless (0) 10/09/21 Day 18 55 Odorless (0) 10/09/24 Day 21 51 Odorless (0)

Drawing. 1 Changes in concentrations of mixed odors in pigs

The second embodiment is tested by an accredited testing institute (Korea Institute of Construction and Environmental Testing) applying the deodorant certification standard (EL.608) and KS I 2218 (2009) among environmental marks under the Act on Environmental Technology Development and Support. It was carried out on request.

First of all, the deodorant certification standard (EL.608) in the environmental mark is divided into quality and sealed spaces from the quality-related standards, and then applied by subdividing it into [basic products for removing odors and acidic odors]. Doing. This is a testament to the fact that existing deodorants are affected by pH, which means that most products are only effective against certain odorous substances. Adsorption agent (X- DEO ) according to the applied technology was confirmed that it is versatile by removing 100% within 90 minutes, regardless of acidity, alkalinity as shown below . Below, the deodorization result of adsorption with the adsorbent of the present invention for four odor components is presented.

Drawing. 2 Ammonia deodorizing ability by time zone

Drawing. 3 Ammonia deodorization graph by time zone

Drawing. 4 Hydrogen sulfide deodorization by time zone

Drawing. 5 Ammonia deodorization graph by time zone

Drawing. Deodorizing ability of methylmercaptan by 6 time zones

Drawing. 7 methylmercaptan deodorization graph by time zone

Drawing. Deodorizing ability of trimethylamine by 8 time zones

Drawing. 9 Trimethylamine deodorization graph by time zone

Adsorbent of the present invention can be used as a deodorant for refrigerators, automobiles, shoe racks, sewer odors, etc. for home use, and it has been confirmed that it has excellent deodorizing ability for volatile organic compounds (VOCs) by removing the sick house syndrome. It can also be used as a product. Industrially, it can be used in odor-causing facilities such as barns, composting factories, environmental foundations, and as an adsorbent for removing gaseous phase (gas phase). This is because the adsorbent of the present invention has excellent versatility (not affected by Ph, less affected by molecular weight, less affected by concentration of odor, less flammable, and less odor controlled in wet places). It is possible to increase the export potential of the product with the ability to surpass the activated carbon which is mainly used as an adsorbent.

Claims (4)

A first step of stirring and crushing the purified sludge;
A second step of mixing and stirring 5 to 15 parts by weight of a material selected from the group consisting of regenerated phosphoric acid and phosphoric acid (or regenerated sulfuric acid and sulfuric acid) and crushed purified water sludge;
A third step of aging the resultant of the second step into the aging tank for 6 to 12 hours while operating the aging tank at regular intervals;
A fourth step of producing a granule-type adsorbent by adding the aged product of the third step to a disk dryer and rotating it while heating to 100 to 200 to adjust the water content to 20 to 40%;
Method for producing a multi-purpose adsorbent, characterized in that A multipurpose adsorbent prepared by the method of claim 1. A first step of stirring and crushing the purified sludge;
A second step of mixing and stirring 5 to 15 parts by weight of a material selected from the group consisting of regenerated phosphoric acid and phosphoric acid (or regenerated sulfuric acid and sulfuric acid) and crushed purified water sludge;
A third step of aging the second step reactant into a aging tank for 6 to 12 hours while operating the aging tank at regular intervals;
A fourth step of producing a granule-type adsorbent by adding the aged product of the third step to a disk dryer and rotating it while heating to 100 to 200 to adjust the water content to 20 to 40%;
A fifth step of granulating the liquid resin with the liquid latex corresponding to 10 to 20% based on 100 parts by weight of the adsorbent through the fourth step and granulating it with an extruder (extruder) heated to 200 to 300;
Method for producing a multi-purpose adsorbent, characterized in that A multipurpose adsorbent prepared by the method of claim 3.

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