KR100423938B1 - A method for filtering method of fibrous compound and an apparatus thereof - Google Patents

Abstract

The present invention relates to a method and apparatus for continuous filtration of fibrous compounds, and more particularly, nozzles and steam, in which a solvent capable of dissolving impurities, is sprayed after a predetermined amount of slurry to be washed and filtered is supported in a filter cell. By repeating the process of passing the sprayed nozzle, washing the impurities by solvent and steam, and simultaneously filtering the waste water in which the impurities are dissolved, and then discharging the filtered product after washing the impurities and filtering the waste water are continuously performed. Therefore, the time required for the washing of impurities and filtration of waste water can be shortened to increase productivity per unit time, improve the quality of products obtained by efficiently reducing the content of impurities, and contribute to environmental conservation by reducing waste water generation. A method and apparatus for continuous filtration of improved fibrous compounds A.

Description

A method for filtering method of fibrous compound and an apparatus

The present invention relates to a method and apparatus for continuous filtration of fibrous compounds, and more particularly, nozzles and steam, in which a solvent capable of dissolving impurities, is sprayed after a predetermined amount of slurry to be washed and filtered is supported in a filter cell. By repeating the process of passing the sprayed nozzle, washing the impurities by solvent and steam, and simultaneously filtering the waste water in which the impurities are dissolved, and then discharging the filtered product after washing the impurities and filtering the waste water are continuously performed. Therefore, the time required for the washing of impurities and filtration of waste water can be shortened to increase productivity per unit time, improve the quality of products obtained by efficiently reducing the content of impurities, and contribute to environmental conservation by reducing waste water generation. A method and apparatus for continuous filtration of improved fibrous compounds A.

Due to the development of the chemical industry, various chemical products are being developed, and efforts to develop products having desired forms and properties by combining or decomposing natural products and chemical products, chemical products and chemical products, or natural products and natural products by constant chemical reactions are continued. It's going on.

After the synthesis of the chemicals, the desired product is obtained and at the same time, impurities generated from side reactions of the base compound remain in the product, which impairs the quality of the product and at the same time causes various problems in the manufacturing process. Since most chemical reactions, the purification of impurities is essentially included in the manufacturing process of the product.

As the purification process, a method of washing the impurities to be removed by using a solvent having a characteristic of dissolving impurities and then filtering the wastewater is frequently used.

Filtration refers to a mechanical operation in which a flowable solid-liquid mixture passes through a porous filter medium, and solids are deposited on the surface or inside of the filter medium, and the liquid is permeated to separate the protons. In a broad sense, this also involves the separation of suspended solids and liquid particles in the gas, but this is generally referred to as filter dust collection, and simply filtration refers to solid-liquid separation operations. Filtration is widely applied in sedimentation and separation in chemical experiments, and is one of the most important unit operations in the chemical industry and other industries. The solid particles are separated from 0.1 to several hundred μm, and the solid concentration is the same as in sand filters. Filtration ranges from extremely dilute to more than 50% slurry. Batch vapor pressure filtration is a common filtration method used in industrial processes.

As a specific example of the use of batch vapor pressure filtration, cellulose ether production method, for example, cellulose ether, which is a very industrially useful compound used as a thickener, binder, and repair agent for medicine, construction, paint, etc., is used as a slurry in the manufacturing process. It is formed into a finished product from which impurities such as salts and glycols are removed through washing and filtration.

Boiling water at about 90 ° C. is added to the synthesized slurry cellulose ether, followed by stirring. At this time, the cellulose ether is evenly dispersed and impurities, such as salt, are completely dissolved in hot water.

Slurry mixed with boiling water is completely transferred to a batch steam pressure filter and filled at 2 kg / cm2 for a period of time to settle the cellulose ether. The stirrer is located at the top of the filter, and the filtered wastewater outlet is filtered in the open state. When the cellulose ether layer appears during filtration, close the outlet, add boiling water at about 90 ℃, fill it at 2kg / ㎠ pressure, open the outlet again, perform second filtration, and then again the cellulose ether surface appears. While rotating the stirrer, it is gradually lowered to the surface and compressed and filtered by a predetermined depth. The stirrer enters the cellulose ether cake and descends to the bottom of the filtration net.

The batch steam pressure filtration method is a widely used method for a manufacturing process that requires not only cellulose ether but also a filtration process. However, since a large amount of water must be used in the filtration process, the filtration time is excessively consumed and impurities such as salt in the product. It is difficult to control the content of and the water content of the filtered product is completed filtration has a problem that it is difficult to obtain a product having a certain physical properties for each synthetic product.

Therefore, it is necessary to consume the processing time and the large amount of water due to the excessive filtration time, which is the problem of the above-described batch steam pressure filtration method. The development of a simple and efficient filtration method that can solve the control problem of the urgent need.

Therefore, the inventors of the present invention improve the batch steam pressure filtration method to support the slurry to be filtered in the filter cell that can be detached from the filter network, and then adjust the amount and pressure of water and the nozzle to spray the steam and around the nozzle is sprayed While rotating at a constant speed, the amount of slurry supported in the filtration cell and the rate at which the filtration cell passes through the nozzle, and the amount and pressure of the water and steam injected through the injection nozzle by controlling the impurity content and It was found that the amount of residual moisture can be controlled. In addition, since the washing of impurities and filtration of wastewater are performed simultaneously, it is possible to shorten the time required for the filtration process and to reduce the amount of wastewater generated by controlling the amount of slurry and the amount and pressure of water sprayed. Completed.

Therefore, the present invention is carried out by repeating the process of passing the nozzle for spraying the solvent and the steam spraying nozzle after dissolving the slurry to be washed and filtered in the filter cell by a predetermined amount to the solvent and steam By the step of washing the impurities and at the same time to filter the waste water in which the impurities are dissolved, the step of discharging the filtered product after washing the impurities and filtration of the waste water is carried out continuously to improve the fibrous compound of the conventional batch vapor pressure filter It is an object to provide a continuous filtration method and a filtration device.

1 is a schematic view showing one embodiment of a rotary continuous filter used in the present invention.

Figure 2 is an enlarged schematic view showing the filtration cell of the rotary continuous filter used in the present invention.

[Description of Major Symbols in Drawing]

10: filter body 12: center rotation axis

14a-14c: solvent spray nozzles 16a-16c: steam spray nozzles

20: filter cell 22: filter network

24: filter network detachable portion 30: slurry input portion

32: filtered product discharge part 34: fruit circulation

36: fruit feeding part 38: fruit discharge part

40: slurry

The present invention provides a method of washing and removing impurities of a fibrous compound and filtering wastewater, the method comprising: 1) supporting a fibrous compound in a filter cell and then rotating the filter cell about a rotation axis; 2) passing the filter cell rotated in the first step through a nozzle in which the solvent is injected; 3) passing the filtration cell through which the solvent is injected in the second step, through the nozzle where steam is injected; And 4) repeating the second and third steps one or more times, and filtering the wastewater while the impurities are washed and removed.

The present invention also provides a device for washing and removing impurities of a fibrous compound and filtering wastewater, comprising: a filter body (10) having a predetermined volume and a thickness; A central rotation shaft 12 mounted in a vertical direction at a central position of the filter body 10 and connected to the motor to be rotatable; A plurality of solvent spray nozzles 14a, 14b, 14c mounted to penetrate the inside of the filter body 10 at equal intervals along the outer circumferential surface of the filter body 10; A plurality of steam spray nozzles (16a) are penetrated with the interior of the filter body (10) at regular intervals along the outer circumferential surface of the filter body (10) and alternately mounted to the solvent spray nozzles (14a), (14b), (14c). , 16b, 16c; The filter network detachable part 24 having a predetermined volume and controlling the height of the slurry 40 to be detached and supported by the filter net 22 is mounted perpendicular to the rotational direction, and is introduced into the slurry input part 30 on one side of the outer surface. A hole in which the slurry 40 may be formed is formed, and a plurality of holes are formed at equal intervals along the left and right directions on the outer diameter surface of the center rotation shaft 12 and are formed at equal intervals in the longitudinal direction of the center rotation shaft 12. Filtration cell 20; A slurry input part 30 formed to allow the slurry 40 to flow through a hole formed at one side of an outer surface of the filtration cell 20; After the solvent spray nozzles 14a, 14b, 14c and the steam spray nozzles 16a, 16b, and 16c have been washed with impurities and the waste water is discharged, A filtered product discharge part 32 through which the filtered product is discharged; Another continuous filtration device of the fibrous compound formed between the outer surface and the inner surface of the filter body 10 and comprising a fruit circulation section 34 and the fruit circulation section 34 in communication with the fruit discharge section 38 It features.

Referring to the present invention in more detail as follows.

The present invention is carried out by repeating the process of passing the nozzle for spraying the solvent and the steam is sprayed to the solvent to dissolve the impurities after supporting the slurry to be washed and filtered in a predetermined amount by the filter cell impurities by the solvent and steam The present invention relates to a method and apparatus for continuous filtration of fibrous compounds in which the step of rinsing and simultaneously filtering the wastewater in which the impurities are dissolved and then discharging the filtered product having been washed with the impurities and filtration of the wastewater is performed continuously.

The continuous filtration method according to the present invention will be described in detail with reference to FIGS. 1 and 2 as follows.

Filter body 10 is rotated about the central axis of rotation (12) and equipped with a plurality of filter cells 20 equipped with a filter net 22, the filter net 22 is a mesh of the net according to the degree of purification of the product It is resizable and can be replaced if necessary.

In the filtration cell 20 rotating at a constant speed, the slurry 40 prepared in the pre-filtration stage is continuously introduced through the slurry input unit 30 to be supported by the filter cell 20 by a predetermined amount, and rotates per unit time. And the amount of the slurry supported by the angle of the filtration cell 20. The filtration cells 20 may be mounted in plural numbers along the outer diameter surface of the center rotation shaft 12, and the number of the filtration cells 20 may vary depending on the circumference of the outer diameter surface of the center rotation shaft 12 and the length of the center rotation shaft 12.

When the filter cell 20 in which the slurry is loaded rotates at a constant speed about the central rotation shaft 12, the slurry 40 and the filter net 22 supported in the filter cell 20 are separated by the centrifugal force generated at this time. Part of the wastewater is filtered. At this time, since the purification efficiency may vary depending on the amount of the slurry 40 to be filled, it is necessary to adjust the input amount and the amount of water to be added according to the product, and it is important to add water at a constant flow rate to achieve uniform filling. Do.

When the rotating filter cell 20 passes through the injection nozzle 14a, which can be sprayed while controlling the amount of water, the salt component, which is an impurity contained in the slurry 40 of the product, is dissolved by the sprayed water. In accordance with the continuous rotational movement, the steam is washed by the pressure injected when passing through the nozzle 16a.

As described above, the wastewater in which the salt component is dissolved is separated and filtered by the centrifugal force and the spray pressure of the water rotating with the filter network 22 mounted on the filter cell 20 interposed therebetween and collecting water pipes under the filter 10. And drained to a separate waste collection tank (not shown) outside the filter.

In addition, in order to maintain the temperature of the slurry to be filtered, the fruit input part 36 and the fruit circulation part 34 communicating with the fruit discharge part 38 are configured inside the outer wall of the filter body 10.

The salt content according to the product is controlled by adjusting the rotational speed of the filtration cell 20 rotating around the central rotation axis 12, or the amount of water used for washing and nozzles 14a, 14b, (the water is sprayed) ( Adjustable by adjusting the injection pressure of 14c). A pressure regulator (not shown) for adjusting the injection pressure of the injection nozzles 14a, 14b, and 14c is similar to the solvent temperature controller (not shown) of the injection nozzles 14a, 14b, and 14c. Preferably near the initial inlet of the solvent.

In addition, according to the fibrous synthetic product used, for example, the process of spraying steam according to various kinds of cellulose ether may be omitted, and the wastewater may be filtered after washing the salt with only the washing water.

In the case of the filtration process, the thickness of the slurry layer 40 filled in the filtration cell 20 can be adjusted by adjusting the position at which the filtration net 22 is mounted, and the layer formed by a conventional batch vapor pressure filtration method. Since it is thin compared to the thickness of the salt, the purification efficiency of the salt is very high, and filtration can be completed in a short time.

According to the continuous filtration method of the present invention, when washing the salt component in the slurry 40 of the product and filtering, the slurry throughput per unit time is preferably 100 to 300 kg, more preferably 150 to 200 kg, At this time, if less than 100 kg productivity per unit time falls, if the throughput exceeds 300 kg waste water generated by the use of excess wash water increases the amount of time is consumed.

The injection pressures of the nozzles 14a, 14b, and 14c into which the washing water is injected are 1 to 5 kg / cm 2, and preferably 1 to 2 kg / cm 2. At this time, if the injection pressure is less than 1kg / ㎠ the filtration effect is lowered, if it exceeds 5 kg / ㎠ filter the product slurry 40 in the filter cell 20, the remaining mass of the product is excessive in the filter network 22 It is compressed and hardened in the form of a lump, which is a problem in the conveying and grinding process.

The filter cell 20 passes through the washing water spray nozzles 14a, 14b, and 14c, and then alternately passes through the nozzles 16a, 16b, and 16c to which steam is sprayed, and thus water content. The rotating filtration cell 20 passes through the nozzles 14a, 14b, 14c, 16a, 16b, and 16c repeatedly while the central rotating shaft 12 is 1. At the point of completing the rotation, the product of the washing of the impurities and the waste water in which the impurities are dissolved are discharged to the outlet 32.

After the filtration process is completed, the product is pulverized to a certain size by the following pulverization process, and then, the size of the pulverized particles is uniformed and then finished.

According to the continuous filtration method of the present invention as described above, the time required for the filtration process can be shortened, so that the time of the entire production process can be shortened, productivity can be improved, and the salt content is 1 to the weight of the dry product. It can be reduced to less than% to improve the quality of the product produced, it is possible to reduce the amount of waste water generated is preferable in terms of environmental conservation while reducing the cost of wastewater treatment.

Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by Examples.

Example 1

8 kg of finely pulverized cellulose was introduced into a high-pressure reactor with a capacity of 100 L, then 10 kg of caustic soda in a 50% aqueous solution was evenly dispersed, and 8 kg of dimethyl ether was added as a diluent to mix evenly. 1 kg and 8 kg of an alkyl halide were added thereto, reacted at 50 to 60 ° C. for 30 minutes, and then heated to 80 to 90 ° C. for 60 minutes to prepare hydroxyalkylalkyl cellulose.

After completion of the reaction, 60 L of hot water was added to the hydroxyalkylalkyl cellulose and stirred, and then the slurry was transferred to the filter in a slurry state, and continuously filtered in the following manner while continuously added to the filter.

Rotating at 10 to 50 RPM, the filter cell in the cylindrical stirrer was filled with 5 kg of the slurry, and then the filter cell was rotated at a predetermined angle (5 to 20 °). The salt (salt) component was sprayed to remove the salt, and steam was sprayed from the secondary nozzle and washed twice to obtain a filtered product from which the salt component was removed.

The filtered product was transferred to a hot air with a pulverizer, dried at the same time as it was pulverized, and filtered to obtain a final cellulose ether. The results of measuring the amount of filtrate used, the time taken for filtration, the viscosity, the salt content, and the amount of wastewater generated were measured. It is shown in Table 1 below.

Example 2:

The same process as in Example 1 was carried out by varying the amount of water used for filtration, and the results are shown in Table 1 below.

Comparative Examples 1-2 :

The same process as in Example 1 was carried out by filtration with a batch steam filter, and the results are shown in Table 1 below.

As shown in Table 1, Examples 1 and 2 performing the filtration step by the continuous filtration method of the present invention 120 to 240 kg / hr treated amount per unit time (the slurry throughput is 200 ~ 500 kg per unit time) / hr), which means that the amount of filtrate treated per unit time in the case of Examples 1 and 2 by the conventional batch pressure filtration method is represented as 30 ~ 32 kg / hr (Slurry throughput 150 ~ 250 kg / hr) The time required for can be reduced by about 4 to 8 times.

In addition, the amount of salt remaining in the finished product was 0.08 to 0.10% in the case of the embodiment of the present invention, while in the comparative example was 2.5 to 3.0%, it can be seen that the removal of the salt was made much higher.

In the embodiment of the present invention, the amount of wastewater generated when treating 60 to 80 kg of the filtrate (slurry) was 75 to 90 kg, whereas the amount of wastewater was 2 to 300 kg in the comparative example. It could be reduced by three times. In other words, the amount of wastewater generated is 5 to 10 weight ratio compared to the synthetic products. This is a breakthrough process compared to the 15-25 weight ratio of the amount of wastewater generated in the conventional batch steam pressure filtration method.

The filtration method according to the present invention can be variously applied not only to the above-described manufacturing process of cellulose ether, but also to an industrial field requiring a purification process.

As described above, according to the continuous filtration method according to the present invention by increasing the throughput of the slurry and the like can be washed and filtered per unit time by reducing the time required for the production process to increase the productivity. Impurities such as salt can be effectively removed to improve the quality of the product and also reduce the environmental waste by reducing the amount of waste water generated.

Claims (3)

In the method of washing by removing impurities of the fibrous compound and filtering the waste water, 1) supporting the fibrous compound in the filter cell and then rotating the filter cell about the rotation axis; 2) passing the filter cell rotated in the first step through a nozzle in which the solvent is injected; 3) passing the filtration cell through which the solvent is injected in the second step, through the nozzle where steam is injected; And 4) filtering the wastewater while the impurities are washed and removed while repeating the second and third steps one or more times. Continuous filtration method of the fibrous compound, characterized in that comprising a. The continuous filtration method of a fibrous compound according to claim 1, wherein the solvent used in the second step is a solvent capable of dissolving impurities to be removed. An apparatus for washing and removing impurities of a fibrous compound and filtering wastewater, the apparatus comprising: a filter body (10) having a predetermined volume and having a thickness; A central rotation shaft 12 mounted in a vertical direction at a central position of the filter body 10 and connected to the motor to be rotatable; A plurality of solvent spray nozzles 14a, 14b, 14c mounted to penetrate the inside of the filter body 10 at equal intervals along the outer circumferential surface of the filter body 10; A plurality of steam spray nozzles 16a which are penetrated with the inside of the filter body 10 at regular intervals along the outer circumferential surface of the filter body 10 and alternately mounted with the solvent spray nozzles 14a, 14b, and 14c. ), (16b), (16c); A filter net detachable part 24 having a predetermined volume and adjusting the detachment of the filter net 22 and the height of the slurry 40 supported thereon is mounted perpendicular to the rotation direction, and flows into the slurry input part 30 on one side of the outer surface. Holes are formed to support the slurry 40 is formed, the equal intervals along the left and right directions on the outer diameter surface of the center rotating shaft 12, and a plurality of mounted at equal intervals in the longitudinal direction of the central rotating shaft 12 Filtration cell 20; A slurry input part 30 formed to allow the slurry 40 to flow through a hole formed at one side of an outer surface of the filtration cell 20; After the solvent spray nozzles 14a, 14b, 14c and the steam spray nozzles 16a, 16b, and 16c have been washed with impurities and the waste water is discharged, A filtered product discharge part 32 through which the filtered product is discharged; Continuous filtering device, characterized in that it is formed between the outer surface and the inner surface of the filter body (10) and comprises a fruit circulation portion 34 and the fruit circulation portion 34 in communication with the fruit discharge portion (38).