JPS5895260A - Separating board - Google Patents

Abstract

PURPOSE:To easily obtain a samll-sized and highly reproducible separating board having the high efficiency of separation to separate each component from a mixture of various compounds, by using a photosensitive glass plate as a base plate and forming the flow passage of fluid on the surface of the base plate by photoetching. CONSTITUTION:A negative mask having a pattern for flow passage 2 shown in the figure is laid on a well-known photosensitive glasspalte (Ex. ''Photoform '' glass manufactured by CORNING GLASS Co. Ltd., in U.S.A.) including photosensitive elements such as gold and silver, and after irradiating ultraviolet rays, the mask is removed and the glass plate is heated at 500 deg.C for 1hr to crystallize the exposed part. After irradiating ultraviolet rays to the whole surface for about 5min, the crystallized part is etched by using 10% hydrofluoric acid to form an etched part on the glass plate 1. Subsequently the etched part is trated with n-dodecanol solution of silane or siloxane to melt and adhere a hard glass plate on the etched surface of the glass plate 1 and the whole is heated at 850 deg.C to obtain a separating board having ceramic construction. Thus a thin, small-sized and highly productive separating board having the high efficiency of separation is obtained.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a separation plate, and particularly to a separation plate using a photosensitive glass substrate suitable for separation of compounds.

Conventionally, separation plates made of glass or metal tubes filled with porous glass powder have been used as a means of separating compounds in each building, based on the principle of stereochromatography. If the separation efficiency is poor and the compounds are difficult to separate, it is necessary to make the tube or tube extremely thin and long in order to increase the separation efficiency. Therefore, this method has the disadvantage that it does not meet the current demands for miniaturization and energy saving, and it also makes it impossible to manufacture products with a fourth separation function with good reproducibility, which separates the same substance. However, the disadvantage is that the conditions for the separation operation must be set for each device.

The present invention relates to a separation plate for separating compounds that solves these disadvantages, and is characterized in that the plate is made of photosensitive glass as a substrate, on the surface of which a fluid flow path is provided by photolithography. be.

To explain this, the present inventors have conducted various studies on separation plates that have good separation efficiency and can be produced at low cost. By forming a fluid flow path using photoetching and using this as a substrate to make a separation plate, we found that a good separation effect could be obtained.As a result of further research on this, we found that it was possible to create a fluid flow path on photosensitive glass. The distribution channel can be formed by using known photographic techniques such as exposure, heat treatment, and etching to obtain a sufficient Mlf, and by doing so, the separation plate can be flattened and miniaturized, and it can also be made with the same shape and performance. The present invention was completed by confirming that it can be obtained extremely easily and with good reproducibility.

The photosensitive glass used as the material for the separator plate of the present invention may be a known one, for example, a combination of silicic acid, Ll,0, KOIN ax
The essential components are alkali or alkaline earth metal oxides such as O, BaO, and photosensitive components such as gold, buttons, and pots, but it also contains CeO2 as necessary.
, a sensitizer such as MnO2, starch as a reducing agent, and alumina as an etching rate improver.

As mentioned above, fluid flow channels are formed on the surface of this photosensitive glass by photo-etching. This is exposed by irradiation with ultraviolet rays, and then heat-treated at 400° C. to 500° C. to crystallize the exposed portion.Q) Then, this portion may be etched with hydrofluoric acid or the like. Note that when producing the negative mask required for this image formation, it is best to design an original in the desired shape that is magnified, for example, 40 to 50 times, and then reduce it. In this case, the entire surface of the material that has been crystallized by heat treatment after exposure is irradiated with ultraviolet rays again, and if necessary, the crystallized portion is removed using hydrofluoric acid or the like. In order to improve the mechanical strength of the image on the retractable glass obtained in this way, the temperature was increased to 700 to 900°C.
It is best to heat treat it to make it into a ceramic.)

The attached drawings show an example of a drawing for producing a separation plate according to the present invention. Figure 1 shows a lath 1 having a photosensitivity as a material, and this is, for example, a rectangular one with sides of It is provided as a gas chromatograph, and one side of it is equipped with four boats for use in gas chromatographs. Figure 2 shows that when reduced, a straight path with a diameter of 02 cm and a length of 90 cm is 0.4-22 mm apart.
It is designed so that five of them are connected in parallel to form a straight section of 20250-. The actual work is to make this enlarged image into a negative mask using the phosphorographic technique, and then print it on the surface of the photosensitive glass.Ultraviolet rays are irradiated from above to print this pattern onto the photosensitive glass. Next, heat this to about 500°C to crystallize this part, and then etch this part with hydrofluoric acid or the like.

The separation plate of the present invention is made by using the photosensitive glass having the image (σ) thus obtained as a substrate, and placing or touching a glass plate on the upper and/or lower surfaces of the photosensitive glass. For example, as can be understood from the 1ilN drawing, it is assumed that a 100-plate body (210,250 m long straight path) can be efficiently separated and purified by the difference in phase molar sensitivity of various compounds. In addition to this, the image can be obtained easily and with good reproducibility by using a negative mask, which has the advantage of controlling productivity.

The separation efficiency of the separation plate of the present invention can be further improved by treating the m-image plane on the photosensitive glass surface with organosilane and/or organosilochitin as described above. This treatment 11 includes, for example, organosilanes such as methyltrimethoxysilane, r-aminopropyltriethoxysilane 1, vinyltrichlorosilane, vinyltriethoxysilane, and hexamethylsilazane, hequinamethyltrisiloxane, and octamethyltetrasiloxane. Examples include organosiloxanes such as various cyclic siloxanes, linear or three-dimensional structured methylpolysiloxanes, methi-terminated phenylpolysiloxanes, and fluorinated ν-rokinanes obtained by fluorinating these. In this treatment, these compounds in the form of liquid, resin, or rubber at room temperature are ripped or made into a solvent solution or emulsion, and the inner surface of the ms on the photosensitive glass surface described above is treated with this, and then dried. A silicone pattern may be formed in this area.

Further, the separating plate of the present invention can be used on the photosensitive glass surface during the above-mentioned organosilane treatment. 1g1. The inner surface is first treated with aminosilane, which is then reacted with nitrobenzene to reduce this nitro group, and then with Na
When diazotized with NOz, this image plane has the function of immobilizing proteins and amino acids, which has the advantage that this separation plate can be applied to the insolubilization of various types of sweets. Given.

Next, examples of the present invention will be given.

Example 100mm x 100mm x 6-photosensitive glass plate
Photoform glass (manufactured by Corning Glass, USA)
A negative mask with the pattern shown in Figure 2 was placed on the product name), and after irradiating it with ultraviolet light for 5 minutes using a 60 ampere arc lamp, the negative mask was removed and heated to 500°C.
This exposed area was crystallized by heat treatment for 1 hour. Next, this entire surface was irradiated with ultraviolet rays for 5 minutes using the arc lamp, and then treated with 10% hydrofluoric acid at room temperature to etch the crystallized parts.
The etched portion shown in FIG. 2I was formed on this photosensitive glass plate.

Next, the etched surface of this photosensitive glass plate (=100IEI
A hard glass plate of 1 x 100 u .

By repeating this operation 6 times, 6 separation plates with the same structure were made, and the etched portions of 5 of them were treated with organosilane or organo-vO xane listed in the following table C2. , using these
Proper tool solution 1 containing 1% each of dodecanol, n-hexadecanol and n-tetradecanol;
When we performed a separation test on this, we obtained the following results.

In addition, the table showing this result shows the inner diameter of 0.3 according to conventional method C;
IIIK, the results of a case where a capillary tube with a length of 50,000 m is spiral (twice wound and used as a separation tube) are also shown as a comparative example, but in this case, the capillary tube is spiral, so the present invention Separation plate C

[Experimental conditions]

Carry gas...Nitrogen separation plate temperature...-110°C to 150°C Heating rate...
...5℃/min [Experimental results] When using these separation plates, n-dodecanol, n-
The relative retention times for hexadecanol and n-tetradecanol = , and in Examples 1 to 6, the separation was good, but in the comparative example, there were many peaks that overlapped, and the separation was insufficient. there were.

In addition, in Examples 1 to 6, the half values of n-dodecanol, n-hequinadecanol, and n-tetradecanol were 2 to 4 times, 3 to 5 times, and 2 to 4 times, respectively, but in the comparative example Now, these will grow to 12 chickens, 15 m, and 11 m.
The separation between each peak was extremely poor compared to that of the example.

table

[Brief explanation of drawings]

FIG. 1 is a plan view of a photosensitive glass used in the layer separation plate of the present invention, and FIG. 2 is a plan view of an enlarged view of a negative mask superimposed on this photosensitive glass. 1...Photosensitive glass, 2.-Ne is a mask patent applicant: Shin-Etsu Chemical Corporation

Claims (1)

[Scope of Claims] 1. Separation plate 2, characterized in that the substrate is a photosensitive glass plate on whose surface a fluid flow path is provided by photo-etching, silane and/or photo-etched photo-sensitive glass. or the separation plate according to claim 881, which is treated with siloxane.