Production of porous glass microbead

[Detailed Description of the Invention]

[Industrial Application] The present invention is a manufacturing process of a porous glass micro bead, and relates to the method of manufacturing a porous glass micro bead simplicity and economically. [Description of the Prior Art] Porous glass micro beads are medicines, such as immobilization support of the carrier for cell cultures, enzyme, or a microorganism, being widely used as the carrier for being impregnated, sustained-release carriers, etc., such as a catalyst carrier and spice, -- what calcinated this at high temperature (about 1000'Q) is known using Si and the milt that is volcanic sediments as the typical manufacturing process. After fusing boro-silicated glass at high temperature, such as 1500degreeC, as the other methods and producing a bead, phase separation is carried out to Na20-B-2O3 phase and 5i02 phase by 500~600 degreeC, the phase which processes from gold ore [ this ] acid and contains B-2 O3 is eluted, and the method of manufacturing porous glass is known. [Problem(s) to be Solved by the Invention] Since high temperature processing of 1000~1500 degreeC is required, each above-mentioned conventional method has a high Energy standard physical unit, and is inconvenient. [ of handling ] Operation of phase separation is needed, especially the above-mentioned latter has a complicated manufacturing process, and it is expensive. It is in the present invention not improving the above-mentioned conventional fault, not carrying out high temperature processing at all, and providing simplicity and the method of manufacturing a porous glass micro bead safely and cheap. [Means for Solving the Problem] The 1st process of the present invention using silicic acid soda as materials, and Granulation(ing) with a spray drier, It is the method of carrying out elution removal of the part for soda in a bead according to the 2nd process of carrying out acid washing of the Granulated material obtained at the 1st process, and also the 3rd process of carrying out alkali washing removing silicic acid sol, and manufacturing a porous glass micro bead simply. [Function] The present invention consists of a thing of the composition like the above, and silicic acid soda is used for it as materials. There is an advantage that it is cheap and can obtain easily, and silicic acid soda is 5iO2-Aj! When aiming at porous glass 203 system, sodium aluminate -- 5i02-Zr02 system and 5102-M2O3-ZrO -- the case where it aims at porous glass 2 system, The solution of a Good luck element and three elements can be freely adjusted to blending zirconic acid soda and sodium aluminate, and zirconic acid soda with silicic acid soda, respectively. The composition per Absolute dry is silicic acid soda 95% and sodium aluminate 5 Chi besides silicic acid soda 100% by this, Various kinds of things, such as silicic acid soda 95 Chi, zirconic acid soda 5%, or silicic acid soda 95 Chi, sodium aluminate 2.5 Chi, and a thing of which zirconic acid soda 2.5 Chi content is done, can be manufactured, and these are chosen suitably as occasion demands. It Granulation with a spray drier by making the above-mentioned silicic acid soda into the 1st process. Although the thing of what kind of publicly known form may be sufficient as the spray drier used for a string, the thing using the centrifugal force which rotates a disk is preferred. In the spray drier of this form, the hollow ball of 10~100-micro particle diameter can be made by adjusting hot wind temperature, the solution speed-of-supply board revolving speed of 2 yen, and solution concentration. Silicic acid soda is formed in the inside ball bead of about 60~80micro of particle diameter in the 1st above-mentioned process, and then acid washing is carried out as the 2nd process. r In this case, using 5 Chi chloride solution etc. as acid to be used, fully agitate a L warming (about 40degreeC) \ bead, and treat it. Acid washing in the 2nd above-mentioned process carries out dissolution removal of the part for the soda in a bead, and the detailed hole of a large number which followed the bead by this is formed. Therefore, in order that acid washing in the 2nd process may fully be eluted in a part for soda and may make a porous body form, it performs acid washing of three Over or more spread good 1. Next, alkali washing is carried out by making into the 3rd process the bead obtained at the 2nd above-mentioned process. Alkali washing removes the acid in the 2nd process to a bowstring, and removes to it the silicic acid sol which arose according to the 2nd process, and fully agitates it in caustic-alkali-of-sodium solution etc. 0.5% to it. 5 and the present invention Granulation this with a spray drier at desired particle diameter using cheap silicic acid soda in materials immediately, furthermore -- since it is what carries out elution removal of the part for the soda in a bead, and is made into a porous body by acid washing -- ° of heat treatment of the conventional Like high temperature -- since it is unnecessary and operation is also easy, as compared with the former, it can manufacture cheap. Since the silicic acid sol which some which were obtained by the above-mentioned method have a possibility that the amount of soda may remain in addition, and arose according to the 2nd process remains, It is preferred to fully wash by a flush and dilute acid washing (for example, 0.5% chloride solution), and to carry out immersion neglect underwater depending on necessity, and it may be Na2O0 and 04 Chi or less by this. As for glass Peace produced by making it above, specific surface area (BET) of 320~430 m 2/and about 0.7~0.9 Bulk specific gravity porosity is acquired for Las micropeace by about 50micro of particle diameter. [Example] The present invention is concretely explained with an example below. Although a drawing is a flow sheet of one example of the present invention, the silicic acid soda which is materials is Granulation(ed) with a spray drier. A spray drier supplies a hot wind so that it may become inlet temperature [ of 175 degrees ] C9 outlet temperature C of 75 degrees, and it is sprayed as number-of-rotations 16.00 Orpm of a disk, and it Granulation it. r Next warm the above-mentioned Granulated product, warm 5 Chi chloride solution to about 40 degreeC, and deal after adding the above-mentioned Granulated product to this and fully agitating to it. In the example, acid washing was repeated 3 times. Granulated product which carried out [ above-mentioned ] acid washing? It adds in O and S S caustic-alkali-of-sodium solution, and agitates enough. In this case, although general machinery churning may be sufficient, when it is good and agitates ultrasonically also by ultrasonic churning, crush of a bead is lessened and the elution removal of the part for soda can fully be carried out. After neglecting the bead which carried out [ above-mentioned ] alkali washing in 4-hour or more pure water after dilute acid washing (about 0.5% chloride solution) Si It was, it r Passed, and also after repeating a flush twice, it dried, and the product was obtained. The 1st table thru/or the 3rd table show composition and physical properties of composition of materials silicic acid soda, the composition after Granulation, physical properties, and the end products, respectively. Each silicic acid soda is JI No. 33 article. 2nd Table Composition after Granulation and Physical Properties (Notes) & Correspond for Materials Silicic Acid Soda to Boil. It is below the same. 3rd Table Composition and Physical Properties [Effect of Invention] of End Products After the present invention's using low Place silicic acid soda as materials and forming microscopic particles with a spray drier like the above, Since a porous glass micro bead can be manufactured by an easy means to carry out acid washing of this, the conventional Like high temperature processing is unnecessary, and the complicated process like phase separation is also unnecessary, and it can reduce cost sharply. The present invention is not limited to manufacture of a porous glass micro bead, but has a porous plate and the advantage that it can manufacture easily, by pouring silicic acid soda into a tabular container, and carrying out after-freeze-drying acid washing.

[Brief Description of the Drawings]

A drawing is a flow sheet of one example of the present invention.