JPS63270516A - Filter sheet for removing microbe and pyrogen in liquid chemical or water - Google Patents

Abstract

PURPOSE:To efficiently and completely remove the microbes and pyrogens in a liq. chemical or water by using the title sheet consisting at least of powdery activated carbon, perlite, and a fiber matrix. CONSTITUTION:Filtration is carried out by using the filter sheet obtained by mixing powdery activated carbon, perlite, and a fibrous matrix, and the microbes and pyrogens in a liq. chemical or water are efficiently removed. In this case, the powdery activated carbon, perlite, and fiber matrix must be uniformly mixed, and hence the sheet having optimum adsorbing and removing performance and filtration quantity is obtained. The amt. of the activated carbon to be added is controlled to >=140%, based on the cellulose fiber which is one component of the fiber matrix, and the amt. of perlite to be added is adjusted to >=70%, based on the cellulose fiber.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a filter sheet for removing microorganisms and pyrogens from a chemical solution or water.

(Prior Art) In the pharmaceutical and medical fields, the removal of microorganisms and pyrogienes from medicinal solutions or water is extremely important and is a frequently performed operation.

Pyrodiene is particularly problematic when it comes to injectable preparations, and when injectables contaminated with this are administered, symptoms such as chills and fever can be seen as side effects. Furthermore, many biological reactions have been reported regarding this pyrodiene, such as vascular effects, bone marrow reactions, cytotoxic effects, anti-inflammatory effects, lethal effects, and endotoxin hypersensitivity. Pyrogen can be considered to be a bacterial endotoxin, and its main component is phospholipid polysaccharide (lipopolysaccharide), and it is said that those from Durham-negative bacteria are particularly pyrogenic.

Conventional methods for removing pyrodiene include heating methods such as high-pressure steam, dry heat, and boiling, filtration methods, irradiation methods such as radiation, ultraviolet rays, and high frequency waves, gas methods such as ethylene oxide and formaldehyde, ethanol, phenol water, formalin water, etc. Chemical liquid methods, etc., are used depending on the purpose and target.

In particular, the filtration method is an operation in which the target sample is simply passed through a porous medium, so there is the least risk of deterioration of the sample.
Therefore, it is often used for liquid media and various liquid pharmaceuticals that contain gases, water, and other soluble and thermally unstable substances.

In addition to the traditional asbestos filtration sheets, diatomaceous earth filtration sheets, electrically charged filtration sheets, etc. are used as filter media for removing microorganisms and pyrogen from the liquid through this filtration.
Recently, methods using "membrane" filter media such as reverse osmosis membranes and ultrafiltration membranes have also been proposed. However, none of these methods is actually satisfactory in terms of removal performance, filtration rate, ease of handling, price, etc. In particular, asbestos filtration sheets are not recommended for use due to medical problems to the human body.

(Problems to be Solved by the Invention) Currently, there is an activated carbon body feed method as a method for removing pyrodiene from medicinal solutions and water that is actually used in the pharmaceutical and medical fields. In this method, a required amount of powdered activated carbon is added to a target liquid such as a chemical solution or water, and after mixing well, the mixture is left to stand for a certain period of time, and the activated carbon that has adsorbed microorganisms and pyrodiene in the liquid is filtered out.

This method is widely used as the most reliable pyrogen removal method.
Although it has been implemented, the following drawbacks have been pointed out.

(b) Operation is batch-type, which is complicated and inefficient.

(II) There is a restriction on the cake collection capacity of the filter.

(c) It is necessary to dispose of used powdered activated carbon, and equipment for this purpose is also required.

(d) The operation of weighing powdered activated carbon and its equipment are necessary, and the working environment is likely to be contaminated because of this.

(f) It is difficult to achieve a complete rose-containing process, and therefore there is a risk of contamination with bacteria, pyrogen, etc. during the manufacturing process. etc., and a pyrogen prevention method that does not have these drawbacks has been desired.

(Object of the Invention) In view of the above points, an object of the present invention is to provide a filter sheet that can more efficiently and completely remove microorganisms and pyrogen in a chemical solution or water by a filtration method. In other words, microorganisms and pyrogens can be removed by filtering chemical solutions or water using a filter equipped with a low-cost filter sheet that has excellent performance in removing microorganisms and pyrogens, has a large throughput, is easy to operate, and has little risk of contaminating the working environment. The purpose is to provide a filter sheet that removes.

(Means for Solving the Problems) The gist of the present invention is that at least powdered activated carbon,
A filtration sheet for removing microorganisms and pyrogens in a chemical solution or water, characterized by comprising perlite and a fiber matrix.

Filter sheets have traditionally been made by mixing diatomaceous earth with cellulose fibers, etc., and have been used for clarification and sterilization filtration, but they are not practical, especially in terms of pyrogen removal performance. Furthermore, sheets made by mixing activated carbon with a fiber matrix have been available for some time, and have been used to decolorize and deodorize colored liquids, but no material has been found that can remove microorganisms and pyrogens in chemical liquids or water by filtration. There wasn't. In view of these points, the inventors of the present invention conducted extensive research, and as a result,
The present inventors have discovered that microorganisms and pyrogens in a chemical solution or water can be efficiently removed by filtering through a filter sheet made by mixing activated carbon and perlite with a fibrous matrix, and have accomplished the present invention.

Activated carbon is a carbon-based material with a large specific surface area and high adsorption capacity that is made by carbonizing wood such as charcoal, palm, sawdust, or coal, and then activating it using a high-temperature steam method or zinc chloride method. It is a substance. In addition to carbon, which is the main component, it also contains constituent elements such as oxygen and hydrogen, and other inorganic components (ash). There are two types of coal, granular coal and powdered coal, with a bulk density of approximately 0.3g/cd and an average pore radius of 1 to 2n1.
), the specific surface area is about 800 to 1500 m''/g.

Activated carbon is generally treated as a hydrophobic (non-polar) adsorbent, and in addition to having the property of selectively adsorbing non-polar substances, it also has functions such as chemisorption ability, catalytic ability, and ion exchange due to the functional groups on the carbon surface. Taking advantage of these properties, it is widely used for decolorizing, deodorizing, purifying, and separating various liquids and gases.

Powdered activated carbon is preferred in the present invention, and is particularly commonly used in
It is preferable to use a highly purified product known as ``pharmaceutical grade'' and low in impurities such as ash. The specific surface area of this powdered activated carbon is 800 to 15001 Ilz/g.

Caramel adsorption amount (JIS-1470) is 85-98%
, methylene blue adsorption amount (JIS-1470) is 12
0~170ml/g s Bulk density is 0.20~0
．． Something around 35 g/cJ is good.

Perlite is a type of filter aid, and pearlite is 800-120
It is heated at 0℃, expanded, crushed, and classified, and its typical composition is SiO□nia 6%, A7z03: 14%, F
ezOz: 0.8%, CaO: 0.8%, MgO
: 0.3%, Ti0z: 0.1%, Na, O: 4%
, KzO: about 5%. Also, the "bulk density" is 0.2~
0.3 g/cd, and the particle size ranges from an average of 1 micron to about 20 microns. For the purpose of the present invention, the particle size is preferably as fine as possible, and the typical particle size distribution is 2.
0 micron or more; 1.8%, 20-10 micron: 3.
8%, 10-5 microns: 14.1%, 5-2 microns 57.8%, 2 microns or less: 22.5%, true specific gravity: 2
．． 2. Bulk density: 0.26 g/crl, pH:
It is 8-9. The matrix fibers are generally natural cellulose fibers, such as refined linter pulp or refined wood pulp such as bleached kraft pulp, but in some cases, inorganic fibers such as glass fibers and various synthetic fibers may also be used.

In general, the degree of freedom of cellulose fibers is preferably 20 to 100 secC10-b in Klemm sedimentation time (pulp concentration: 0.1%). A long settling time is effective in preventing the movement and falling off of powdered activated carbon and perlite in the filter sheet, and also increases the filtration efficiency and strength of the sheet.

Generally, cellulose fibers are beaten alone and then mixed with activated carbon and perlite, but in some cases, they may be mixed with activated carbon and perlite in advance and then beaten together. In any case, it is necessary that the powdered activated carbon, perlite and fiber matrix be uniformly mixed to obtain a sheet with optimum adsorption and removal performance and filtration rate. The amount of activated carbon added must be 140% or more based on the cellulose fiber, and is generally 160 to 240%.
% is most preferable. On the other hand, the amount of perlite added is 70% or more, preferably 80 to 1% of the cellulose fiber.
It is about 20%. In order to increase sheet strength or further increase adsorption properties, it is also possible to add a cationic polymer compound such as polyamide epichlorohydrin condensate in an amount of about 0.5 to 5.0% based on the total amount of solids. It is.

It is also possible to use pearlite that has been cationically modified in advance with these cationic polymer compounds.

The thickness of the filtration sheet of the present invention is 3 to 9 yen per filtration chamber,
In particular, 4 to 8 fins are good. If the thickness is too thin, the liquid permeation channel will be too short and adsorption will tend to be incomplete, and if the thickness exceeds 101), there is a risk of "edge leakage". Usually, one sheet is used for each filtration chamber, but in some cases, two or more thin sheets may be laminated to obtain the desired thickness. Also, the weight of the sheet is 1700~2 per filtration chamber.
000 g/m", and the water transport rate at that time is 10 to 30 seconds per 100 mA' of water, especially 20
Preferably about sec.

If it is 60 seconds or more, the filtration speed is too high and is not practical, and if it is too fast, 10 seconds or less, the voids in the sheet become large and the adsorption time is insufficient.

In order to prevent activated carbon and perlite particles from falling off the filter sheet during handling and filtration work, fine cellulose fibers, glass fiber filter paper, or precision It is also possible to protect the porous sheet filter medium 3 such as a filter membrane by attaching relatively coarse filter paper or a non-woven sheet such as non-woven fabric to the downstream side thereof.

At this time, there are various adhesive materials such as liquid and solid, but heat-melting nonwoven fabrics such as polypropylene are particularly preferred from a sanitary standpoint. It can be attached by placing a heat-fusible fibrous nonwoven fabric on top of the filter sheet, and then placing the above-mentioned protective sheet on top of it and applying light heat pressure.

A pressure filtration machine is generally used as a filtration device, but the filter sheet of the present invention has a support porous part that can stably support it, a seal part such as a packing is perfect, and there is no risk of "spillage". It is necessary that the Considering the intended use, stainless steel is preferable as the material.

(Example) Hereinafter, the present invention will be specifically explained by giving examples of manufacturing a filter sheet of the present invention and a filter sheet for comparison, and then giving test examples.

Example 1 Two types of filter sheets according to the present invention and three types of filter sheets of Comparative Examples having the compositions shown in Table 1 were produced by the following method.

Add the required amount of cellulose fiber to a beater filled with water at approximately 1%.
After disintegration, lower the beater blade to beat to the specified cream freeness, raise the beater blade, add the specified amount of activated carbon and auxiliary agents, and stir well to mix and use as papermaking raw material. . Using this papermaking raw material, a filtration sheet having a thickness of 5 to 71 mm and a dry weight of 1500 to 1800 g/m2 was produced using a vacuum hand-sheet machine and dried at 105 DEG C.

Test Example 1 Pyrodiene-containing deionized water and 0.9% saline were filtered using the filter sheet shown in Example 1, and their removal ability and removal capacity were measured. The results are shown in Table-2.

Measurement conditions: Test solution: Deionized water and 0.9% saline containing Ecolt LPS 2.5 ng/ml Filtration area: 50 d Filtration rate: 3cIII/l1in Pyrogen detection method: Limulus method (LimulusAm
ebocyte Lysate Te5t).

Symbols in the table: (W): Pyrodiene-containing deionized water (S): 0.9% saline 10: Pyrodiene reaction present - None ±: Slightly present Test Example 2 Filter sheet shown in Example 1 above Pyrodiene-containing deionized water and 0.9% saline were filtered at various filtration speeds, and changes in pyrodiene removal ability were investigated. The results are shown in Table-3.

Measurement conditions: Same as Test Example 1 except for filtration rate.

Symbols in the table: (W): Pyrogen-containing deionized water (S): 0.9% saline +: Pyrogen reaction 1: None ± 2 Slightly present 3 Major case 3 Produced according to Example 1 above Using the filtration sheet 2 of the present invention, various test solutions having different pyrodiene concentrations as shown in Table 4 were filtered, and the pyrodiene removal performance in each case was investigated.

Measurement conditions: Filtration rate = 2c! l/1Ilin, other than this test example 1
Same Table-4 N, D: Not detected (W): Pyrodiene-containing deionized water (S): 0.9% saline Table-5 (Effects of the invention) As explained in detail above, the filtration sheet of the present invention can be used in chemical solutions. This is a new and practical filtration sheet for microorganisms and pyrogens, which not only can efficiently remove microorganisms and pyrogens in water, but also has no risk of contaminating the working environment and has a large throughput, and is beneficial for medical and pharmaceutical applications. It is extremely large.

[Brief explanation of the drawing]

FIG. 1 is a schematic cross-sectional view of a filter sheet of the present invention, and FIG. 2 is a schematic cross-sectional view of a filter sheet of the present invention with porous sheets pasted on both sides. Patent applicant: Toyo Roshi Co., Ltd. and one other person Figure 1 Figure 2

Claims (2)

[Claims] (1) A filtration sheet for removing microorganisms and pyrogens in a chemical solution or water, characterized by comprising at least powdered activated carbon, perlite, and a fiber matrix. (2) A filtration sheet for removing microorganisms and pyrogens in a chemical solution or water as set forth in claim 1, which is obtained by pasting porous sheets on both sides of the filtration sheet.