JP2001113165A - Adsorbent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a porous adsorbent excellent in adsorptivity and which is hardly changed with time by forming a porous cement hardened body containing a zeolite-like material from a cement slurry mixed with a powdery or granular mineral material consisting essentially of silica and alumina. SOLUTION: A cement slurry consisting of 70-150 pts.wt. water, based on 100 pts.wt. cement, and 5-50 pts.wt. powdery or granular mineral material with silica and alumina as the main components is formed. The slurry is successively cured at atmospheric pressure and high temperature, and then cured at high pressure and high temperature and made porous to obtain the adsorbent.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a cement slurry having a specified water content, in particular, an inexpensive raw material such as waste cement slurry, and the adjustment of the water content and the functionalities such as adsorption capacity and ion exchange capacity. Additives and porous adsorbents obtained by two-stage curing. More specifically, purifying wastewater, river water, air, etc. as an environmental material utilizing the excellent adsorption function caused by the porous structure. Purifying materials that enhance the function,
Underfloor humidity control materials, humidity control deodorant wall materials, heat insulation / sound absorption boards, panels, building materials that make up a comfortable living space, greening, medium materials, soil improvement materials, civil engineering and agricultural materials that improve the environment for plant growth, etc. The present invention relates to an adsorbent suitably used for

[0002]

2. Description of the Related Art While industrial development has helped improve people's lives, it has caused pollution that threatens people's lives. Knowing that this pollution will cause inhumane damage to humans, humanity has begun to move towards a new goal of improving lives without pollution.

[0003] Water pollution in rivers, lakes, oceans, and the like is considered to be a typical pollution along with air pollution. To prevent this water pollution, a certain amount or more of wastewater is discharged to rivers, lakes, oceans, and the like. Although water quality is regulated for companies and other companies, water quality is not regulated for general household wastewater, which has a relatively small amount of wastewater.

[0004] This water quality regulation has achieved certain results,
The water quality of lakes, marshes, oceans, etc. has been improved compared to at one time. In particular, it can be evaluated that strict water quality regulations on the emission of heavy metals and poisons that cause deterioration or loss of physical function have considerably improved the safety of water quality of rivers and the like. However, it is said that water pollution due to drainage from unregulated wastewater sources has not declined, but rather is intensified. Have been.

[0005] The most important of these water quality problems in rivers, lakes, marshes, and oceans is "Aoko", which causes damage to the fishery.
And the problem of eutrophication causing red tide. That is,
The problem is that the content of organic matter, nitrogen compounds, phosphoric acid and phosphate in water becomes too large.

[0006] Organic sewage such as animal urine sewage, household wastewater, and sewage are widely known as eutrophication of water quality. In order to prevent eutrophication of water quality, a method for treating these organic sewage is used. Have been proposed.

[0007] For example, sewage is subjected to preliminary treatment such as screen, sand settling, sedimentation and the like to separate solid (sludge) from liquid, and then subjected to high-grade treatment such as sprinkling filtration method and activated sludge method to be oxidized. Thereafter, the biological treatment, the final precipitation (or sedimentation), and the disinfection are sequentially performed.

[0008] The screen is a process of flowing sewage through a parallel bar, grid, or mesh sieve, and merely mechanically removing coarse suspended matters in the sewage. Sedimentation reduces the flow rate of the sewage and removes heavy solids. This is the treatment to precipitate the gravel. In the sedimentation treatment, in order to separate the organic matter to be subjected to a post-treatment different from that of the sand and gravel from the sand and gravel, the flow rate is adjusted so that the organic matter is not precipitated as much as possible.

[0009] Precipitation includes ordinary precipitation and chemical precipitation, and ordinary precipitation mainly precipitates organic suspended matter. This precipitate is called settled sludge or raw sludge. Chemical precipitation is a method of causing flocculation and sedimentation by adding a chemical in order to promote sedimentation of sludge. The chemical used is a sulfate band, aluminum chloride, trivalent or divalent iron sulfate, iron trichloride, Representative examples include iron chloride, slaked lime, and organic flocculants.

[0010] The chemical precipitation can remove 80 to 95% of the suspended solids, so it was thought that the sewage treatment was even solved by this. However, the septicity of the effluent sewage, the amount of precipitated sludge was increased, and the cost of chemicals was high. With the big problem of
At present, it can be said that it has been replaced by biological processing in high-grade processing.

The sprinkling filtration method is typical of the biological treatment, in which sewage is sprayed on a coarse filter medium in a fountain form and adhered to the surface of the filter medium while the sewage flows downward through the gaps of the coarse filter medium. This is a treatment method in which the aerobic cell membrane is touched and oxidized, and there are a fixed method in which the watering position is fixed, and a rotating method in which the watering position is rotated by using the reaction of watering. This sprinkling filtration method has advantages such as easy maintenance and low manpower, good oxidation of sewage effluent, and no spoilage.

In the activated sludge method, when the sewage is sufficiently stirred with oxygen, the sludge becomes spongy and has a large volume.
This is a treatment based on the fact that it easily precipitates when it is allowed to stand. If the sludge generated in this way is returned to about 25% and mixed with new sewage, work will be extremely clear in a short time. A good supernatant can be obtained.

Meanwhile, in recent years, a porous calcium silicate-based one has been proposed as a microorganism carrier used for denitrification and dephosphorization (see Japanese Patent Publication No. 6-83832).

This microorganism carrier is obtained by subjecting a foamed hardened material obtained by foaming a water slurry composed of a siliceous raw material and a calcareous raw material in the presence of a foaming agent to a hydrothermal reaction, and
The main component is porous calcium silicate having a porosity of 90%. ], And as the siliceous raw material,
Powders of silica sand, cristobalite, amorphous silica, diatomaceous earth, ferrosilicon, clay, etc. "are used, and as the calcareous material," powder of quicklime, slaked lime, cement, etc. "is used. As the foaming agent, "a metal foaming agent such as aluminum powder or a foaming agent such as an AE agent" is used. As the foaming agent, specifically, "resin soaps, saponins, synthetic surfactants" , Hydrolyzed proteins, polymeric surfactants and the like ".

[0015] Examples of porous calcium silicate hydrates as products include CHS gel, tobermorite, and zonolite.

In the water treatment using the microbial carrier, the organic wastewater, which has been subjected to primary treatment to remove suspended matters and precipitates, is passed through an aerobic filter bed tank filled with the filter medium without dilution while being aerated. Thus, the removal of organic substances by the biofilm method, the removal of phosphorus, and the nitrification of nitrogen compounds are simultaneously performed. Then, in order to treat the treated water containing the nitrified nitrogen compound, the treated water is introduced from the aerobic filter bed tank into the anaerobic filter bed tank, and a hydrogen donor such as methanol is added thereto, whereby the gas is passed through the anaerobic filter. In this state, biological denitrification is performed by denitrifying bacteria.

The size of the microorganism carrier is 0.5
It is considered that 10 to 10 mm is desirable.

On the other hand, improvement of water quality by using a porous material such as charcoal or zeolite as a filter medium has been performed for a long time. For example, a technology for removing the smell of tap water by attaching a water purifier filled with activated carbon to a faucet of a domestic water supply and passing the water flowing out of the faucet through the water purifier has already been put into practical use.

[0019]

In the conventional microorganism carrier, since a water slurry comprising a siliceous raw material and a calcareous raw material is foamed in the presence of a foaming agent, the pore size is reduced. There is a problem that unevenness is caused, and the adsorption ability of microorganisms, the treatment ability of sewage, and the durability vary, making it difficult to produce a uniform product.

In addition, waste materials are not used as raw materials but are purchased as raw materials, which increases material costs and requires equipment and labor for forming the water slurry. However, considering the equipment costs and labor costs, it must be expensive.

Further, 0.5 to 10 which is considered to be desirable
With a particle size of mm, if it is used as a purification material for river water, it may be washed away by a water flow.

In addition, to carry out nitrification of organic substances, phosphorus and ammonia nitrogen by a biofilm, it is necessary that a certain number of microorganisms inhabit the microorganism carrier, and the microorganisms are implanted on the microorganism carrier. It has a major drawback in that it can hardly be expected to have a purification function during breeding beyond a certain level.

On the other hand, charcoal and zeolite adsorb organic matter, phosphate ions and ammonia nitrogen in the treated water due to their chemical and physical adsorbing ability. Because of its low properties and strength, there is a problem that if it is used as a purification material for river water, it will be washed away or damaged.

In order to solve this problem of strength, for example, it is conceivable to mix zeolite into concrete. However, since concrete itself is a highly water-tight material, the effect of zeolite exposed on the surface can be expected. ,
There is a problem that the zeolite buried inside cannot be expected to work.

[0025] In the meantime, while the conventional technology for improving water quality using a porous body has these technical problems, a cement product manufacturing plant using cement such as concrete pile as a raw material inevitably requires cement. In some cases, waste cement slurries containing such wastewater are generated, and there is a problem that expensive treatment costs must be spent for treating the waste cement slurries.

For example, in a concrete pile manufacturing process, cement milk is put into a cylindrical mold, and the mold is rotated around its axis and centrifugally formed. In order to reduce this, it is necessary to discharge the slurry-like cement waste material at the center outside the formwork.

In the fume tube manufacturing process, cement milk is charged into a cylindrical mold, and the mold is rotated around its axis and centrifugally formed. In order to maintain the dimensional accuracy of the above, it is necessary to discharge the slurry-like cement waste material at the center outside the formwork.

Slurry-like cement waste material generated in a plant for producing these concrete piles and fume pipes,
In other words, the waste cement slurry hardens when left to stand,
The cured product has a low strength, and there is a concern that the disintegration proceeds with the passage of time and that the alkaline component is eluted, thereby affecting the environment.

Further, the cured product of the waste cement slurry cannot be strengthened even by steam curing, and cannot be reused as a structural material.

Therefore, it has been studied to solidify waste cement slurry into blocks of a certain size and use it as a landfill material. However, it is interpreted that it is difficult to put the waste cement slurry to practical use because of these problems. After all, waste cement slurries have so far been expensively disposed of as industrial waste.

Therefore, in order to solve the problem that a large treatment cost is required, while studying the effective use of the waste cement slurry for some purpose, the components of the waste cement slurry are composed of components of cement and water. Except that the weight ratio is almost 1: 1, it is found that Portland cement and silica fine powder are the main components, and the mineral composition and pore distribution change over time with hydrate formation and crystal growth. did.

Therefore, the inventor of the present invention has set that the weight ratio of water to cement (referred to as water cement weight ratio) of ordinary cement hardened material is 50 in order to use waste cement slurry as an effective resource. % Or less, the ratio was increased to manufacture an adsorbent, and a water purification test was performed using the obtained various adsorbents. In particular, the weight ratio of water cement was as large as 70 to 150%. Forming a cement slurry, filling the mold in a mold frame, and performing normal pressure and high temperature curing (steam curing) to obtain a porous body having a relatively uniform pore diameter of calcium hydroxide and calcium carbonate, It has been found that when the porous body is cured at a high temperature and a high pressure (autoclave curing) following the normal pressure and a high temperature curing, a porous cured body having no change with time can be obtained.

Further, the porous cured body has a porous structure having fine pores continuous by calcium silicate hydrate called CSH gel or tobermorite gel in which calcium hydroxide and silica are combined, In addition, it was found that in addition to the calcium silicate hydrate, a hydration product containing calcium and alumina as main components was contained.

Further, when the porous body cured by normal-pressure and high-temperature curing is cured at high temperature and high pressure, a hydrothermal reaction occurs. This hydrothermal reaction suppresses alkali elution and increases the strength of the cured product. The hydration product of the alumina component generated by this hydrothermal reaction has a similar function to zeolite, and has excellent adsorption capacity for environmental pollutants such as phosphoric acid, phosphate, and nitrogen compounds that enrich water quality. It was found to have.

In addition, the porous cured product has a pore volume of 0.2 to 0.75 mL / g and a specific surface area of 15 to 55 m ² / g.
g and very large pores, and these pores have a maximum pore radius of 0.05 to 0.45 μm, and there are widely different pore radii or diameters of submicron or less. Of course, the diameter 20 ~
Many pores of 500 angstroms (called mesopores) are also included.

The cement slurry contains CaO /
In the presence of a silica component having a SiO ₂ molar ratio of 2.0 or less, CaO forms calcium silicate hydrates such as tobermorite and zonotlite from the silica component and water, and is a zeolite-like substance, that is, alumina. It was also found that the formation of a hydrated product with bound components did not progress.

From this, the inventors of the invention according to Japanese Patent Publication No. 6-83832 suggested that the porous calcium silicate-based microbial carrier according to the present invention has CaO / SiO ₂
Molar ratio = 0.5-2.0, specifically 0.8, 1.0,
Since the siliceous raw material and the calcareous raw material are blended so as to be 1.5, the silica content is CaO / SiO ₂ molar ratio =
If it exceeds 2.0, it is interpreted that it was not possible to know that a zeolite-like substance was produced, and it was not possible to know that this zeolite-like substance could be produced. It is interpreted that the idea that the mineral substance has a function of purifying water by absorbing environmental pollutants could not be reached.

In the invention according to Japanese Patent Publication No. 6-83832, a direct attention is paid to biological treatment, and a foaming agent is used to form pores suitable for implantation and propagation of microorganisms. It is presumed that the technical means of making it porous was adopted.

According to the present invention, as described above, a cement slurry having a water cement weight ratio of 70 to 150% and a powdery or granular mineral material containing silica and alumina as main components is usually used. It has been completed based on the finding that a porous cured body containing a zeolite analog can be obtained by curing under high pressure and high temperature after curing under high pressure and high temperature. Cement hardener containing a zeolite analog is formed from a cement slurry containing a powdery or granular mineral material containing aluminum and alumina as main components. In addition to exhibiting extremely excellent adsorption function for nitrogen compounds, it has excellent ion exchange capacity for adsorption of microorganisms and various ions such as phosphate ions. Exhibits functions such as air purification, humidity control / odor control, heat insulation / sound absorption, soil improvement / modification, etc., and also has the long-term stability and durability of these various functions. It is an object to provide an adsorbent.

[0040]

In order to achieve this object, an adsorbent according to the present invention comprises 70-150 parts by weight of water and 100 parts by weight of cement and powder containing silica and alumina as main components. A cement slurry comprising 5 to 50 parts by weight of a granular or granular mineral material, which is subjected to normal-pressure and high-temperature curing and high-pressure and high-temperature curing in that order to obtain a hardened and porous structure. .

Water 70 to 100 parts by weight of cement
150 parts by weight and 5 to 50 parts by weight of a powdery or granular mineral material containing silica and alumina as main components are mixed and kneaded to form a cement slurry, which is then put into a mold and then subjected to normal pressure. When high-temperature curing is performed, a porous body having a composition of calcium hydroxide and calcium carbonate having a relatively uniform pore diameter due to evaporation of water is obtained. Subsequently, when this porous body is cured under high pressure and high temperature, a zeolite analog is obtained. Can be obtained.

The obtained adsorbent is porous with little change over time, exhibits a remarkably excellent adsorption function for nitrogen compounds such as ammoniacal nitrogen, and adsorbs microorganisms and phosphate ions. Exceptional ion exchange capacity for various types of ions, air and other purification functions, humidity control and deodorant functions,
It can exhibit heat insulation / sound absorption function, soil improvement / modification function, etc., and can provide a porous hardened material (adsorbent) which is extremely excellent in long-term stability and durability of these various functions, and is extremely inexpensive. It is.

In other words, the porous cured product, that is, the adsorbent according to the present invention contains a hydration product similar to zeolite, and eutrophizes water such as organic substances, phosphoric acid, phosphates, and nitrogen compounds. Demonstrates excellent adsorption and retention of water polluting substances and air pollutants such as odorous components in the air, moisture in the air, metal ions such as phosphate and potassium ions and ammonium ions in the soil, and moisture. Therefore, it is extremely useful as an adsorbent used for purification and improvement of rivers, lakes, marshes, oceans, air, soil, and the like.

Hereinafter, the adsorbent of the present invention will be described in more detail. The cement used in the present invention is not particularly limited, and a commercially available cement is desirable from the viewpoint of production cost, availability, and the like.

This cement includes Portland cement,
Portland cements include mixed cements and specialty cements. Portland cements include ordinary Portland cement, early-strength Portland cement, ultra-high-strength Portland cement, moderate heat Portland cement, low heat Portland cement, sulfate-resistant Boltland cement, A low alkali type in which the total alkali is suppressed to 0.6% or less is included.

The mixed cement is obtained by binding a suitable quenching blast furnace slag or bozolan material to Portland cement clinker and pulverizing, and includes blast furnace cement, silica cement, and fly ash cement.

As a representative of the special cements, bauxite is mixed with an approximately equal amount of limestone, melt-fired, and then quenched and ground. An ultra-fast-hardening cement which shows enhancement and can be expected to have high strength can be given.

Of these cements, the cheapest,
It is recommended to use ordinary Portland cement which is easily available.

The powdery or granular mineral material containing silica and alumina as main components used in the present invention is not particularly limited as long as it produces a zeolite analog in the two-stage curing step. However, a fly ash that produces the least expensive zeolite analog with the best adsorption capacity is desirable.

In order to obtain the adsorbent according to the present invention, first, a powdery or granular mineral material 5 containing 70 to 150 parts by weight of water and silica and alumina as main components with respect to 100 parts by weight of cement. ~ 50 parts by weight are blended and kneaded to form a cement slurry.

If the amount of water is less than 70 parts by weight with respect to 100 parts by weight of cement, the porosity due to evaporation of water is limited, and it is difficult to obtain an adsorbent exhibiting the required adsorption capacity. Exceeding parts by weight may result in separation of materials, difficulty in curing even after two-stage curing, and decrease in the strength of the cured body. From these viewpoints, it is particularly desirable to use 75 to 125 parts by weight of water with respect to 100 parts by weight of cement.

If the amount of the powdery or granular mineral material containing silica and alumina as main components is less than 5 parts by weight with respect to 100 parts by weight of cement, formation of a zeolite analog is insufficient and desired adsorption On the other hand, if it exceeds 50 parts by weight, the effects of various functions such as adsorption are limited, and it is not only meaningless to add more than that, but the cured product (adsorbent) )) Is not preferred because of the possibility of lowering the strength.
It is preferable to use 10 to 30 parts by weight of a powdery or granular mineral material containing silica and alumina as main components with respect to 00 parts by weight.

The obtained cement slurry is put into a mold, and then subjected to normal pressure and high temperature curing. When the cement slurry has a relatively uniform pore diameter due to evaporation of water, it has a porous composition of calcium hydroxide and calcium carbonate. When a porous body is obtained, and then the porous body is cured under high pressure and high temperature, a porous cured body (adsorbent) containing a zeolite analog can be obtained.

Here, the normal pressure and high temperature curing for curing the cement slurry put into the mold is performed in the same procedure as the well-known steam curing, and it takes a proper time to bring the cement from room temperature to a predetermined curing temperature. After the temperature of the slurry is raised, the curing temperature is maintained for a predetermined time and then the slurry is allowed to cool in the air. The curing temperature is not particularly limited, and the curing time for maintaining the curing temperature is not particularly limited. For example, the curing temperature may be 60 to 75 ° C., and the curing time for maintaining the curing temperature is 5 ° C. It should be about an hour.

Further, the cement slurry is hardened by normal pressure and high temperature curing, and a porous body having a relatively uniform pore diameter and having a composition of calcium hydroxide and calcium carbonate is obtained. Thus, a porous cured body (adsorbent) with little change over time can be obtained.

The high-pressure and high-temperature curing is performed using an autoclave at a temperature of 160 to 180 ° C. and a pressure of 8 to 10 kg / cm ² for about 4 hours.
For the cooling after the high-pressure and high-temperature curing, for example, a method of cooling to about 120 ° C. in about 3 hours, water cooling to about room temperature in about 4 hours, and then cooling to room temperature by natural cooling is adopted. Is done.

The cured product (adsorbent) thus obtained
Contains a CSH gel in which calcium hydroxide and siliceous matter have not changed with time, and contains a hydration product containing calcium and alumina as main components.

Further, due to the hydrothermal reaction that proceeds during the high-pressure and high-temperature curing, alkali elution from the cured product (adsorbent) is suppressed, and the strength of the cured product (adsorbent) is increased. In addition, the hydration product to which the alumina component formed by the hydrothermal reaction is combined has a function similar to zeolite, that is, for example, has a physical adsorption ability, phosphoric acid,
It exhibits excellent adsorption capacity for environmental pollutants that enrich the water quality such as phosphates and nitrogen compounds. In this case, microorganisms are adsorbed on the cured product (adsorbent), and an excellent denitrification effect can be obtained by the microorganism adsorption.

In the present invention, the method of forming the cement slurry is not particularly limited, but the material cost is reduced and the waste cement slurry generated during the production of the cement product is effectively used. It is desirable to improve the environment by using it as an effective resource.

That is, in the adsorbent according to the present invention, water or cement or a powdery or granular mineral material containing silica and alumina as main components is added to waste cement slurry generated during the production of a cement product. Unit weight 1.
It is preferable to adjust the pressure to ³ to 1.7 t / m ³ , and perform a normal pressure and high temperature curing and a high pressure and high temperature curing in order to obtain a cured and porous structure.

By the way, water or cement or a powdery or granular mineral material containing silica and alumina as main components is added to a waste cement slurry generated during the production of a cement product to obtain a unit volume weight of 1.3 to 1. The reason for adjusting to 7 t / m ³ is that by adjusting to this range, the same adsorbent as the adsorbent can be obtained with the same component ratio as in the case of the adsorbent according to the present invention.

That is, the inventor of the present invention has found that waste cement slurry has no use, requires a great deal of cost for its treatment, and also causes environmental degradation. During the research on its effective use in some applications, the components of waste cement slurry consisted mainly of Portland cement and fine silica powder, except that the weight ratio of cement and water was almost 1: 1. Thus, it was found that the mineral composition and the pore distribution change over time with the formation of hydrates and crystal growth.

In order to use waste cement slurry as an effective resource, the present inventor has set the weight ratio of water (hereinafter referred to as water cement weight ratio) to cement of a normal hardened cement material to 50. % Or less, the ratio was increased to manufacture an adsorbent, and a water purification test was performed using the obtained various adsorbents. In particular, the weight ratio of water cement was as large as 70 to 150%. Forming a cement slurry, filling the mold in a mold frame, and performing normal pressure and high temperature curing (steam curing) to obtain a porous body having a relatively uniform pore diameter of calcium hydroxide and calcium carbonate, Following the normal pressure and high temperature curing, it was found that if the porous body was cured at high temperature and high pressure (autoclave curing), a porous cured body with little change with time could be obtained. .

The porous cured body has a porous structure having fine pores continuous by calcium silicate hydrate called CSH gel or tobermorite gel in which calcium hydroxide and silica are combined, In addition, it was found that in addition to the calcium silicate hydrate, a hydration product containing calcium and alumina as main components was contained.

Further, when the porous body cured by normal-pressure and high-temperature curing is cured at high temperature and high pressure, a hydrothermal reaction occurs. This hydrothermal reaction suppresses alkali elution and increases the strength of the cured product. The hydration product of the alumina component generated by this hydrothermal reaction has a similar function to zeolite, and has excellent adsorption capacity for environmental pollutants such as phosphoric acid, phosphate, and nitrogen compounds that enrich water quality. It was found to have.

The porous cured material (adsorbent) has a pore volume of 0.2 to 0.75 mL / g and a specific surface area of 15 to
There are very many pores of 55 m ² / g, and these pores have a maximum pore radius of 0.05 to 0.45 μm, and those having sub-microns or less and having widely different pore radii or diameters exist. I have. Of course, many pores (called mesopores) having a diameter of 20 to 500 angstroms which are considered to be involved in the adsorption are included.

The waste cement slurry generated during the production of this cement product is a cement product manufacturing plant using cement such as concrete pile as a raw material.
A waste cement slurry containing cement may inevitably occur, and this waste cement slurry may be mentioned.

More specifically, for example, in a concrete pile manufacturing process, cement milk is put into a cylindrical mold, and the mold is rotated around its axis and centrifugally molded. In order to reduce the weight of the product, a waste cement slurry in which a slurry-like cement waste material at the center is discharged outside the formwork may be used.

In the fume tube manufacturing process, cement milk is put into a cylindrical mold, and the mold is rotated around its axis to form a centrifugal mold. In order to protect the dimensional accuracy of the waste cement waste, a waste cement slurry in which a slurry-like cement waste material at the center is discharged outside the formwork may be used.

In the present invention, after the above-mentioned cement slurry is formed, this cement slurry is poured into a mold. The shape of the mold chamber of the mold is not particularly limited. Any shape such as a rectangular shape including a plate shape, a cylindrical shape, a fan shape, an L shape, an H shape, a conical shape, a triangular pyramid shape, a quadrangular pyramid shape, and a tetrapot shape can be selected. Alternatively, an appropriate core may be arranged in the mold chamber to form a hollow cured product such as a cylinder, a square tube, or a cubic frame.

Further, in the present invention, a mixture of 5 to 50 parts by weight of a functional aggregate having an adsorbing function with respect to 100 parts by weight of cement in a cement slurry has an adsorbing function of the obtained adsorbent. This is advantageous in further improving the treatment capacity of the adsorbent of the present invention.

Examples of the functional aggregate include at least one selected from porous mineral materials such as zeolite, zeolitic tuff, porous iron oxide and perlite, activated carbon and rice husk charcoal.

The functional aggregate used in the present invention includes phosphoric acid,
There is no particular limitation as long as the granules have an adsorbing function for environmental pollutants such as phosphates and nitrogen compounds that enrich the water quality, but zeolites having physical adsorbing ability are considered in view of price and availability. It is recommended to use an activated carbon material such as zeolite analogs such as zeolites and zeolitic tuffs, or rice husk charcoal having chemical adsorption ability.

The preferred amount of the functional aggregate depends on the functional aggregate used. For example, in the case of zeolite tuff, the weight ratio to cement is 10 to 40%.
In the case of chaff charcoal, the weight ratio to cement is preferably 5 to 15%.

When the present invention is formed in a pebble shape or formed in a cobblestone shape and placed on a riverbed or a riverbank, before the present invention is poured into a mold, it is prevented from being washed away by a water current. Preferably, the aggregate is mixed and kneaded with the cement slurry so that the specific gravity after hardening is 2.5 to 3.5.

That is, it is desirable that the adsorbent according to the present invention is one in which an aggregate such as iron ore is blended into a cement slurry so that the specific gravity is 2.5 to 3.5.

The aggregate for the purpose of adjusting the specific gravity naturally needs to have a specific gravity of more than 2.75, particularly, a specific gravity of more than 3. For example, coarse aggregate made of iron ore is required. What is necessary is just to use a fine aggregate or fine aggregate, or to use a coarse aggregate and a fine aggregate made of these iron ores in combination.

The mixing of the aggregate into the cement slurry is as follows:
It is also useful for preventing cracks from occurring during the solidification stage, such as during normal pressure and high temperature curing and during high pressure and high temperature curing. The type of aggregate for the purpose of preventing the crack is not particularly limited, and for example, an aggregate made of silica stone, tuff, or the like, which is mixed with ordinary mortar or concrete as an aggregate may be used.

Among them, it is more preferable to use an aggregate made of tuff, which does not cause settlement cracks on the casting surface and has an adsorption ability. However, settlement cracks on the casting surface caused when the aggregate made of silica stone is mixed can be eliminated by placing the aggregate and the slurry in a mold and then performing vibration compaction. Even in the case where the settlement cracks sometimes occur on the casting surface, the occurrence of the settlement cracks can be prevented by performing the vibration compaction in the same manner.

The method of mixing the aggregate with the cement slurry is not particularly limited. For example, a method of mixing the aggregate with the cement slurry in advance, kneading the mixture, and then pouring the mixture into the mold may be employed. After filling the aggregate such as silica stone and tuff, the method of pouring the slurry into the mold, the method of putting the aggregate into the mold in which the cement slurry is poured first, and the like are adopted. You can do it.

However, when the cement slurry is put into the mold after the aggregate made of tuff is filled in the mold, the aggregate may rise. In order to solve this problem, tuff is used as the aggregate. When used, it is desirable to adopt a method in which the aggregate and the slurry are mixed, kneaded and mixed (after premixing), and then the mixture is poured into a mold.

The adsorbent according to the present invention can be fiber-reinforced to increase bending strength and compressive strength. However, in this case, it is preferable that the lower surface of the mold chamber and the side of the casting surface be reinforced in the same manner. For example, when the surface of the adsorbent is fiber-reinforced, it is preferable that both the lower surface of the mold chamber and the casting surface (or the upper surface of the mold chamber) be fiber-reinforced, and only the casting surface (or the upper surface of the mold chamber) or the mold. If only the lower surface of the room is fiber-reinforced, cracks may occur during normal pressure and high temperature curing, which is not preferable.

The material of the fiber used for fiber reinforcement is not particularly limited, but it is preferable to use an inorganic fiber such as a carbon fiber and a steel chip. Further, the length of the fiber used for fiber reinforcement is not particularly limited, and may be a long fiber or a short fiber. In addition, these fibers can be knitted into cloth,
They may be woven or used, bonded to a non-woven fabric or mat shape with a binder, used, bundled or knitted in a rope shape, or used separately. Among the use forms of these reinforcing fibers, the form used by bonding them in a nonwoven fabric or mat shape with a binder is inexpensive, easy to handle, and furthermore, from the viewpoint that the reinforcing fibers can be arranged evenly. desirable.

However, in the case of using a binder in which fibers are bonded in a nonwoven fabric or mat shape with a binder, the binder may melt during high-pressure and high-temperature curing and precipitate on the surface during cooling. Alternatively, the fibers themselves may melt and precipitate on the surface during cooling. In particular, when using a glass fiber nonwoven fabric or a glass fiber mat having a relatively low fiber melting point, it is necessary to set a low curing temperature and set a long curing period in order to prevent the binder from dissolving. Problems arise.

Since the carbon fiber mat has a binder dissolution temperature higher than the curing temperature during the high-pressure and high-temperature curing of the cement slurry, there is no problem of dissolution and precipitation of the binder, but the cement slurry hardly penetrates and the cured product is hardened. Fibers may be exposed on the surface of the glass. However, this problem does not occur if the slurry is poured into the mold, vibration compaction is performed, and the cement slurry is sufficiently permeated between the fibers before curing.

[0086]

As described above, the adsorbent according to the present invention is a powdery or granular mineral material containing 70 to 150 parts by weight of water and silica and alumina as main components with respect to 100 parts by weight of cement. A cement slurry consisting of 5 to 50 parts by weight is formed, and is cured by sequentially performing normal pressure and high temperature curing and high pressure and high temperature curing to form a porous structure, so that a hydration product having a function similar to zeolite, That is, it is a porous hardened product containing a hydration product to which an alumina component is bound, and which does not change with time, and thereby, an organic substance, phosphoric acid, a phosphate, an environmental pollutant that enriches water quality such as a nitrogen compound. The effect of exhibiting an excellent adsorption ability to the odor is obtained.

In the present invention, a cement slurry is prepared by adding water or cement or a powdery or granular mineral material containing silica and alumina as main components to a waste cement slurry produced in a cement product manufacturing process. When formed by adjusting the unit volume weight to 1.3 to 1.7 t / m ³ , a dedicated facility for producing a cement slurry becomes unnecessary, and the labor for producing a cement slurry can be greatly reduced. And the like.

Further, in the present invention, a mixture of 5 to 50 parts by weight of a functional aggregate having an adsorbing function with respect to 100 parts by weight of cement in a cement slurry is used to reduce environmental pollutants of the obtained adsorbent. The effect of further improving the adsorption function and significantly increasing the treatment capacity of the adsorbent of the present invention can be obtained.

Here, the use of inexpensive and easily available materials such as natural mineral materials and rice husk charcoal containing silica and alumina as the main components as the functional aggregate can further reduce the raw material cost. Is obtained.

In addition, in the present invention, when an aggregate made of, for example, iron ore is added to the cement slurry so that the specific gravity after hardening becomes 2.5 to 3.5, the specific gravity of the present invention becomes It is the same as the specific gravity of the cobblestone placed on the riverbed and riverbank for protection of the riverbank and the riverbank, it can be prevented from being washed away by the flowing water force, and it can be laid on the riverbed and riverbank by simple work of simply throwing it into the water Is obtained.

Although the present invention was originally invented as an adsorbent used for water purification and air purification, it has an adsorbing ability, and therefore, after adsorbing a fertilizer, a soil conditioner or the like in advance, or Without adsorbing soil or soil improvement materials, they can be sown on the ground or buried in the soil to green,
The effect of being able to be used as an agricultural material, a horticultural material, or a civil engineering material that improves the cultivation environment of plants, such as a culture medium and soil improvement, is obtained.

Further, since the present invention has an adsorbing ability, it can be used as a building material such as a humidifier under the floor and a humidifying and deodorizing wall material. Further, since the present invention is porous, it can be used as a heat insulating material and a sound insulating material. It can be used as a building material such as, for example, and by using these building materials, it is possible to obtain an effect of increasing the comfort of a living space.

[0093]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be specifically described with reference to the drawings, but the present invention is not limited to these embodiments.

Example 1 An adsorbent according to one example of the present invention was formed using a cement slurry composed of waste cement slurry discharged from a mold after centrifugal formation of a concrete pile and stored in a container. is there.

In this concrete pile, 100 parts by weight of ordinary Portland cement, 50 parts by weight of water, and 50 parts by weight of coarse aggregate made of silica are mixed and kneaded, and the mixed concrete milk is put into a mold room of a formwork. It is formed by centrifugal molding by pouring and rotating the mold together with the center axis of the mold chamber. In order to reduce the weight, waste cement slurry collected at the center during the centrifugal formation is taken out.

When the waste cement slurry stored in the container is adjusted with cement, fly ash, and water so that the unit volume weight of the waste cement slurry is about 1.5 t / m ³ , 10 parts by weight of fly ash is added to 100 parts by weight of cement. Parts.

Then, after confirming that the unit volume weight of the waste cement slurry was about 1.5 t / m ³ , FIG.
As shown in the flow diagram, the diameter is 50 mm, the depth is 30 mm
The waste cement slurry is poured into a mold having a cylindrical mold chamber, and left for 1 hour, followed by curing under normal pressure and high temperature.

As shown in the temperature control characteristic diagram of FIG. 2, the waste cement slurry rises to about 27 ° C. by the heat generated by the hydration reaction started after the mixing of the raw materials,
In this normal pressure and high temperature curing, the slurry is heated from this temperature (about 27 ° C.) to 70 ° C. over about 3 hours, and then heated to 60 ° C.
The test was performed while maintaining the temperature in a range of 75 ° C. and an average temperature of 70 ° C. for about 4 hours.

[0099] By the curing under normal pressure and high temperature, the waste cement slurry is hardened to obtain a porous hardened body having a composition of calcium hydroxide and calcium carbonate (hereinafter referred to as a porous body).

Next, this porous body was mixed with the concrete
Put in an autoclave at the same time as the pile and cure under high pressure and high temperature
You. The temperature of the porous body before placing in the autoclave
Decreases to 35-43 ° C., but the temperature control characteristic line of FIG.
As shown in the figure, in the high pressure and high temperature curing, this porous
The body is raised from this temperature to 165-180 ° C over 3 hours
While the furnace pressure is at normal pressure
9 to 10 kg / cm ^TwoAfter raising the pressure to
65-180 ° C, average 175 ° C, furnace pressure 9-10K
g / cm^Two9.8 Kg / cm on average^TwoHold for 4 hours
To reduce the road pressure to normal pressure in two and a half hours
The furnace temperature was raised to about 120 ° C over 3 hours by forced air cooling.
Temperature and then 4 hours with water cooling.
After cooling to 20 ° C, the porous body and
And slowly reduce the furnace temperature to room temperature. And this porous body
After the mold is cooled down to room temperature,
The formed adsorbent can be obtained. More
Also crush the adsorbent thus formed into a filter medium
It is also possible to use it. Thus, the adsorption of the present invention
Wood was obtained.

By the way, due to the hydrothermal reaction that proceeds during the high-pressure and high-temperature curing, alkali elution from the adsorbent is suppressed and the strength of the adsorbent is increased. In addition, the hydrothermal reaction generates a CSH gel in which calcium hydroxide and siliceous are bonded in the adsorbent and a hydration product in which alumina is bonded.

Since this hydration product has countless fine pores, it has a function similar to zeolite, that is, it has a physical adsorption ability and, as described later, an organic substance, phosphoric acid, a phosphate, a nitrogen compound. It exhibits excellent adsorption capacity to environmental pollutants that eutrophication of water quality.

Example 2 Further, in a mold to which the waste cement slurry, that is, the waste cement slurry discharged from the mold in the concrete pile manufacturing process, was added in advance to 100 parts by weight of the cement in the waste cement slurry. , 40 parts by weight of an aggregate made of zeolite tuff was filled as a functional aggregate. Thereafter, the waste cement slurry was poured into a mold having a cylindrical mold chamber, and then subjected to vibration compaction. After this,
A porous hardened body in which a functional aggregate made of zeolite tuff is arranged on the surface by sequentially performing normal pressure and high temperature curing and high pressure and high temperature curing in the same manner as in Example 1, and then releasing the mold. Was obtained.

Example 3 Next, in the waste cement slurry, that is, the waste cement slurry discharged from the mold in the concrete pile production process, 100 parts by weight of the cement in the waste cement slurry was mixed with rice husk charcoal. Weight parts as a functional aggregate, knead and mix, then pour this mixture into the mold,
In the same manner as in Example 1, a normal pressure and high temperature curing and a high pressure and high temperature curing are sequentially performed, and then a mold release is performed to form a porous cured body in which a functional aggregate made of chaff charcoal is blended. An adsorbent was obtained.

These Embodiments 1, 2, and 3
For these, an adsorption ability test of ammonia nitrogen, orthophosphoric phosphorus, and a pesticide (isoprothiolane) was performed in the following manner. The ion exchange capacity of each of the powders obtained by crushing Examples 1, 2 and 3 was measured.

In the ammonia nitrogen adsorption ability test, the initial concentration of ammonia nitrogen was 70 mg / L, 20 mg / L,
And 1 mg of each test solution were adjusted with ammonium sulfate (special grade of reagent) so as to be 5 mg / L, and Example 1, Example 2 and Example 3 were immersed in separate 1 L test solutions in a lump, and stirred. 0 hours, 4 hours, 2 hours with gentle stirring
The concentration of ammonia nitrogen after 4 hours was measured by indophenol blue absorption spectrophotometry, and the removal rate was calculated.

As a result, as shown in Table 1, Table 2, Table 3, FIG. 4, FIG. 5, FIG. 6, FIG. 7, FIG.
After 24 hours, the removal rate of ammonia nitrogen reached 49% to 74%, and the removal rate at the high concentration level (70 ppm) was the medium concentration level in the order of Example 2> Example 1> Example 3. It was found that the removal rate of (20 ppm) was in the order of Example 3> Example 2> Example 1, and the removal rate of the medium concentration level (20 ppm) was in the order of Example 1> Example 2> Example 3.

[0108]

[Table 1]

[0109]

[Table 2]

[0110]

[Table 3]

[0111] In the test for the ability to adsorb orthophosphate phosphorus, 1 L of a test solution was adjusted with potassium dihydrogen phosphate (special grade reagent) so that the concentration of orthophosphate phosphorus became 50 mg / L and 5 mg / L. Each of Examples 1, 2 and 3 was immersed in a 1 L test solution in a lump in a test solution in a lump state, and orthophosphoric phosphorus at 0, 4 and 24 hours after gently stirring with a stirrer. The concentration was measured by molybdenum blue absorptiometry and the removal was calculated.

As a result, Tables 4 and 5, FIGS.
As shown in FIGS. 12 and 13, the high concentration level (50 pp) was used.
m), the removal effect is low at 13.3 to 32.7%, but the removal ratio at the low concentration level (5 ppm) is 90.0 to
An extremely high removal effect is observed at 98.6%. In each case, the order of Example 3> Example 2> Example 1 is the same, and it is recognized that the removal rate of Example 1 is slightly lower than those of the other examples.

[0113]

[Table 4]

[0114]

[Table 5]

In the test for the ability to adsorb pesticides, a test solution having a concentration of 2 mg / L was prepared by diluting isoprothiolane (a standard solution of 1000 mg / L acetone) with acetone to prepare a test solution having a concentration of 2 mg / L. And Example 3 was immersed in a separate test solution in a lump, and stirred gently with a stirrer.
The concentration of the residual pesticide after 24 hours and 24 hours was measured by GC / MS, and the removal rate was calculated.

As a result, as shown in Table 6, FIGS. 14 and 15, it was confirmed that the isoprothiolane removal rate after 24 hours in each example was 20 to 30%. In addition,
It can be seen that the removal rate of Example 2 was slightly lower than the other examples.

[0117]

[Table 6]

The ion exchange capacity (CEC) was measured by placing 20 g of the powder obtained by crushing Examples 1, 2 and 3 in 100 mL of an ammonium acetate solution and allowing them to stand overnight, and then filtering the solution. The residue is washed with methanol. The washed residue was subjected to displacement extraction of ammonium ion (NH ₄ +) with a 10% sodium chloride solution, and the ammonia ion (NH ₄ +) was analyzed by neutralization titration to determine the ion exchange capacity.

As a result, as shown in Table 7, the ion exchange capacity of Example 2 was the largest, followed by Example 3 and Example 1. The ion exchange capacity of the third embodiment is about three times that of the first embodiment.

Incidentally, it can be said that there is not much correlation between the ion exchange capacity and the ammonia nitrogen absorption capacity.

[0121]

[Table 7]

In the above Examples 2 and 3, a functional aggregate was mixed with the slurry. However, for example, iron ore was added to the slurry together with or instead of the functional aggregate. The specific gravity of the present invention can be adjusted by mixing an aggregate made of stone. When this specific gravity adjusting aggregate is blended and the specific gravity of the present invention is adjusted to about 3.0,
The present invention has a specific gravity similar to that of a cobblestone, and can prevent the present invention charged in running water from being washed away by the force of the water flow.

[0123]

As described above, the adsorbent according to the present invention is characterized in that 70 to 15 parts of water is added to 100 parts by weight of cement.
A cement slurry comprising 5 to 50 parts by weight of a powdery or granular mineral material containing 0 parts by weight and a silica component and an alumina component as main components is formed and cured by sequentially performing normal pressure and high temperature curing and high pressure and high temperature curing. Since it has a porous structure, a porous cured body containing a zeolite analog is formed, and the action of this zeolite analog allows ammoniacal nitrogen,
As a result of being able to adsorb and remove water contaminants such as orthophosphoric phosphorus and pesticides, the adsorbent of the present invention is introduced into rivers, lakes and marshes, drainage facilities, etc., and is laid, so that water flowing therethrough and stored there. This has the effect of improving the water quality by removing the water pollutants from the existing water and purifying the water.

However, the adsorbent according to the present invention is formed in a block shape and laid as a protective material on the floor of a river or on the bottom of a lake, as a protective material on the shore, or as a protective material on the shore. It is also possible to remove water contaminants from water in contact with the adsorbent of the present invention, which constitutes a part of these revetment materials, revetment materials or framework revetment, to improve water quality, The effect of purifying can be obtained.

Further, the adsorbent according to the present invention contains a zeolite analog, and by its function, adsorbs nitrogen oxides, sulfur oxides, odorous components and the like in the air and purifies the air. Thus, an effect that can be used as an adsorbent for air purification is obtained.

Furthermore, since the adsorbent according to the present invention is porous, it can be used as a building material for improving the comfort of living space, such as a floor conditioning material, a moisture conditioning material, a deodorant wall material, a heat insulating material, and a sound absorbing material. The effect that can also be used is obtained.

In addition, since the adsorbent according to the present invention is a porous hardened material containing a zeolite analog, a pre-adsorbed fertilizer or soil conditioner can be diffused in the soil or can support nutrients in the soil. The effect that it can be utilized also as agricultural material, horticultural material, or civil engineering material which raises soil strength.

In the present invention, waste cement slurry produced in the production process of cement products can be used instead of using new materials such as cement. In this case, the waste cement slurry produced during the production of cement products can be used. When water or cement or a powdery or granular mineral material containing silica and alumina as main components is added to the waste cement slurry to be adjusted to a unit volume weight of 1.3 to 1.7 t / m ³ , the waste cement slurry Water-cement ratio of 70-150
%, And the component ratio is within the required range described above, and this is cured by sequentially performing normal pressure and high temperature curing and high pressure and high temperature curing to form a porous structure, thus requiring no special equipment and labor. Therefore, it is possible to use the waste cement slurry, which has been treated as industrial waste, effectively as a raw material of the present invention. An effect that can be significantly increased is obtained.

In the present invention, the adsorbing ability can be increased by blending a functional aggregate with the cement slurry. For example, 10 to 40% by weight to cement
When a functional aggregate made of zeolite tuff is mixed, the effect of increasing the adsorption ability of ammonia nitrogen and orthophosphate phosphorus can be obtained. Also, when a functional aggregate composed of rice husk charcoal in a weight ratio of 5 to 15% with respect to cement is added to the slurry, it is possible to obtain an effect of increasing the adsorbing ability of a medium concentration level of ammonia nitrogen and orthophosphate phosphorus. it can.

Further, in the present invention, when an aggregate having a large specific gravity, for example, an aggregate made of iron ore, is blended with the cement slurry so that the specific gravity of the hardened material becomes 2.5 to 3.5, the adsorption according to the present invention is achieved. The specific gravity of the material is the same as that of natural cobblestone in water, and an effect of preventing the adsorbent of the present invention from being washed away by the water force can be obtained.

[Brief description of the drawings]

FIG. 1 is a flowchart of a manufacturing process of the present invention.

FIG. 2 is a temperature control characteristic diagram of normal pressure and high temperature curing according to the present invention.

FIG. 3 is a temperature control characteristic diagram of the high-pressure and high-temperature curing of the present invention.

FIG. 4 is a high concentration level ammonia nitrogen concentration change characteristic diagram of the present invention.

FIG. 5 is a characteristic diagram of a medium-concentration level ammoniacal nitrogen concentration change characteristic of the present invention.

FIG. 6 is a low concentration level ammonia nitrogen concentration change characteristic diagram of the present invention.

FIG. 7 is a characteristic diagram of a high-concentration level ammonia nitrogen removal rate according to the present invention.

FIG. 8 is a characteristic diagram of a medium-concentration level ammonia nitrogen removal rate of the present invention.

FIG. 9 is a characteristic diagram of a low-concentration level ammonia nitrogen removal rate according to the present invention.

FIG. 10 is a concentration characteristic diagram of a high-concentration level orthophosphoric phosphorus of the present invention.

FIG. 11 is a concentration characteristic diagram of a low-concentration level orthophosphoric phosphorus of the present invention.

FIG. 12 is a characteristic diagram of a high-concentration level orthophosphoric phosphorus removal rate of the present invention.

FIG. 13 is a characteristic diagram of the removal rate of low-concentration orthophosphoric phosphorus according to the present invention.

FIG. 14 is a concentration characteristic diagram of the isoprothiolane of the present invention.

FIG. 15 is a characteristic diagram of the removal rate of isoprothiolane of the present invention.

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Claims (5)

[Claims] 1. 100 parts by weight of cement and 70 parts by weight of water
To 150 parts by weight and 5 to 50 parts by weight of a powdery or granular mineral material having silica and alumina components as main components, and sequentially performing normal pressure and high temperature curing and high pressure and high temperature curing. An adsorbent characterized by having a cured, porous structure. 2. A waste cement slurry generated during the production of a cement product is charged with water or cement or a powdery or granular mineral material containing silica and alumina as main components, and has a unit volume weight of 1.3 to 1. An adsorbent characterized by being adjusted to 7 t / m ³ , and then being cured by normal pressure and high temperature curing and then high pressure and high temperature curing to form a porous structure. 3. The adsorbent according to claim 1, wherein 5 to 50 parts by weight of a functional aggregate having an adsorption function is blended with 100 parts by weight of cement in the cement slurry. 4. The functional aggregate comprises at least one selected from the group consisting of zeolite, zeolitic tuff, porous mineral materials such as porous iron oxide and perlite, activated carbon and rice husk charcoal.
The adsorbent according to any one of claims 1 to 3, which is a seed. 5. An adsorbent in which an aggregate such as iron ore is blended into a cement slurry such that the specific gravity of the adsorbent according to any one of claims 1 to 4 is 2.5 to 3.5. .