CN113264688A - Sectional coating device and method for inner surface of quartz capillary column - Google Patents
Sectional coating device and method for inner surface of quartz capillary column Download PDFInfo
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- CN113264688A CN113264688A CN202110685067.3A CN202110685067A CN113264688A CN 113264688 A CN113264688 A CN 113264688A CN 202110685067 A CN202110685067 A CN 202110685067A CN 113264688 A CN113264688 A CN 113264688A
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- capillary column
- quartz capillary
- coating
- coated
- temperature
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- 239000010453 quartz Substances 0.000 title claims abstract description 70
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000576 coating method Methods 0.000 title claims abstract description 63
- 239000011248 coating agent Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 30
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 15
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000002103 nanocoating Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 24
- 230000032683 aging Effects 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 239000011043 treated quartz Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Devices For Use In Laboratory Experiments (AREA)
Abstract
The invention discloses a sectional coating device and a method for the inner surface of a quartz capillary column, which comprises the steps of cleaning the inner surface of the quartz capillary column to be coated by using an alkane reagent, wherein the cleaning pressure is 0.1-0.3 MPa; dissolving the polymer stationary phase to be coated by an alkane reagent machine, wherein the dissolving concentration is 0.1-0.25 mg/mL, and the polymer stationary phase is used after being fully dissolved; after the quartz capillary column to be coated is inserted into the sectional coating device, the solution of the fully dissolved stationary phase is pressed into the quartz capillary column under the preset pressure, and two ends of the quartz capillary column are sealed; the inner surface of the quartz capillary column is fully adhered with the high molecular coating, the distance between two adjusting plates of the sectional coating device is adjusted to be the same as the preset distance, the coating temperature and the coating time of the sectional coating device are set, and high-temperature coating is carried out; after the high-temperature coating is finished, the quartz capillary column is washed by alkanes to remove the high-molecular stationary phase which is not heated by the high-temperature coating.
Description
Technical Field
The invention relates to the technical field of quartz capillary column manufacturing, in particular to a device and a method for sectionally coating the inner surface of a quartz capillary column.
Background
The quartz capillary column is a thin tube which is coated with a polyimide protective layer on the surface of quartz, has elasticity and can resist high temperature of about 400 ℃, and has the diameter of 0.1mm, 0.25mm, 0.32mm, 0.53mm and the like and the length of 15 meters, 30 meters, 60 meters and the like. After the inner surface is coated with a layer of high polymer (stationary phase) with different chemical properties and different thicknesses, the gas chromatographic column becomes a gas chromatographic column used in the field of gas chromatographic analysis, and is mainly used for analyzing gas and material components capable of being gasified at high temperature.
The quartz capillary column is generally coated with different kinds of polymer coatings (stationary phases) on the inner surface according to different analyzed material components, and in the manufacturing process, the polymer stationary phases are generally synthesized first, and then the inner surface of the whole quartz capillary column is coated with different kinds of coatings with different thicknesses (0.1, 0.25, 0.32 and 0.53 microns) through a plurality of process means.
In current manufacturing processes, all are high molecular coatings applied to the inner surface of the entire tube length of a quartz capillary column, but for some specific analytical applications, a high molecular coating of a specified length (typically 5-10 cm) is applied to the middle or a specified location of the entire tube length, which requires a specific coating apparatus and method.
Disclosure of Invention
1. The technical problem to be solved is as follows:
aiming at the technical problems, the invention provides a sectional coating device and a sectional coating method for the inner surface of a quartz capillary column, which can coat a polymer coating with a preset length on the middle or a certain specified position of the quartz capillary column.
2. The technical scheme is as follows:
a sectional coating device for the inner surface of a quartz capillary column comprises an adjustable heating box; the method is characterized in that: the adjustable heating box is provided with two adjusting plates capable of moving left and right; a heating pipe is arranged between the adjusting plates which move left and right; a cavity between the left and right adjusting plates forms a closed heating space, and a section to be heated of the quartz capillary column to be coated is suspended in the heating space; through holes capable of penetrating through a quartz capillary column to be coated are formed in the side wall of the adjusting heating box and the corresponding positions of the adjusting plate which moves left and right; an ultrasonic ranging unit for measuring the distance between the adjusting plates moving left and right is arranged between the adjusting plates moving left and right; also includes a control unit; the control unit comprises a singlechip, a temperature control circuit and a clock circuit; the temperature control circuit, the clock circuit and the ultrasonic ranging unit are all connected with the single chip microcomputer, and heating temperature control, heating time control and distance control between the adjusting plates of the heating space are achieved respectively.
Furthermore, the adjusting plate moving left and right is driven to move left and right by a servo motor arranged outside the adjustable installation box; an output shaft of the servo motor is connected with the screw rod to drive the screw rod to move; the screw rod drives the adjusting plate to move left and right; the motor control circuit is connected with the single chip microcomputer to realize the control of the motor.
Furthermore, a temperature sensor is arranged in the closed heating space; the temperature sensor transmits the acquired information to the singlechip.
Further, the device also comprises a liquid device and a liquid pump; the liquid in the liquid device is pumped into the inner cavity of the quartz capillary column to be coated by a liquid pump; and the control circuit of the liquid pump is connected with the singlechip.
A sectional coating method for the inner surface of a quartz capillary column is characterized in that: the method comprises the following steps:
the method comprises the following steps: the quartz capillary column to be coated is cleaned with alkane reagent at the inner surface pressure of 0.1-0.3 MPa.
Step two: dissolving the polymer stationary phase to be coated by an alkane reagent machine, wherein the dissolving concentration is 0.1mg-0.25mg/mL, and the polymer stationary phase is used after being fully dissolved.
Step three: after the quartz capillary column to be coated is inserted into the sectional coating device, the solution of the sufficiently dissolved stationary phase is pressed into the quartz capillary column under the preset pressure, and two ends of the quartz capillary column are sealed.
Step four: the inner surface of the quartz capillary column is fully adhered with the high molecular coating, the distance between two adjusting plates of the sectional coating device is adjusted to be the same as the preset distance, the coating temperature and the coating time of the sectional coating device are set, and high-temperature coating is carried out.
Step five: after the high-temperature coating is finished, the quartz capillary column is washed by alkanes to remove the high-molecular stationary phase which is not heated by the high-temperature coating.
Step six: and aging for a preset time, and then taking down the treated quartz capillary column.
Further, the third step further comprises the step of leading out the stationary phase solution in the quartz capillary column after being sealed is attached for 24 hours.
3. Has the advantages that:
(1) the scheme adopts a method for adjusting the heating space of the heating box to realize the control of different lengths of different sections of the quartz capillary tube, the adjusting plate which moves left and right is arranged in the adjustable heating box, the quartz capillary tube column of the section to be coated is suspended in a high-temperature space, when coating is carried out, only the quartz capillary tube column of the section to be coated is heated, the heated section to be coated can realize the coating of the stationary phase, and other parts pass through the stationary phase liquid but do not pass through the heating, and the inner surface of the other parts is not coated by the stationary phase liquid. In order to adapt to the coating requirements of different stationary phase liquids, a temperature sensor is arranged in a heating box to acquire temperature information in a heating space to a single chip microcomputer, a clock circuit is arranged to control heating time, and an ultrasonic ranging unit is arranged to acquire the distance between two adjusting plates, so that the automatic control of the whole coating process is realized. In order to pour the stationary phase liquid smoothly, the device adopts a liquid pump to transfer the stationary phase liquid into the quartz capillary column to be coated, and then the two ends of the quartz capillary column are sealed.
(2) The scheme provides a coating method for the segmented coating device, the quartz capillary column to be coated is directly arranged on the segmented coating device in the method, the processes of coating, aging and the like can be realized only by the segmented coating device, and the use is convenient.
Drawings
FIG. 1 is a cross-sectional view of an adjustable heating chamber of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
As shown in fig. 1, a sectional coating apparatus for an inner surface of a quartz capillary column comprises an adjustable heating chamber; the method is characterized in that: the adjustable heating box is provided with two adjusting plates 1 which can move left and right; a heating pipe 2 is arranged between the adjusting plates which move left and right; a cavity between the left and right adjusting plates forms a closed heating space, and a section to be heated of the quartz capillary column 3 to be coated is suspended in the heating space; through holes capable of penetrating through a quartz capillary column to be coated are formed in the side wall of the adjusting heating box and the corresponding positions of the adjusting plate which moves left and right; an ultrasonic ranging unit for measuring the distance between the adjusting plates moving left and right is arranged between the adjusting plates moving left and right; also includes a control unit; the control unit comprises a singlechip, a temperature control circuit and a clock circuit; the temperature control circuit, the clock circuit and the ultrasonic ranging unit are all connected with the single chip microcomputer, and heating temperature control, heating time control and distance control between the adjusting plates of the heating space are achieved respectively.
Furthermore, the adjusting plate moving left and right is driven to move left and right by a servo motor 4 arranged outside the adjustable installation box; an output shaft of the servo motor is connected with the screw rod 5 to drive the screw rod to move; the screw rod drives the adjusting plate to move left and right; the motor control circuit is connected with the single chip microcomputer to realize the control of the motor.
Furthermore, a temperature sensor is arranged in the closed heating space; the temperature sensor transmits the acquired information to the singlechip.
Further, the device also comprises a liquid device and a liquid pump; the liquid in the liquid device is pumped into the inner cavity of the quartz capillary column to be coated by a liquid pump; and the control circuit of the liquid pump is connected with the singlechip.
A sectional coating method for the inner surface of a quartz capillary column is characterized in that: the method comprises the following steps:
the method comprises the following steps: the quartz capillary column to be coated is cleaned with alkane reagent at the inner surface pressure of 0.1-0.3 MPa.
Step two: dissolving the polymer stationary phase to be coated by an alkane reagent machine, wherein the dissolving concentration is 0.1mg-0.25mg/mL, and the polymer stationary phase is used after being fully dissolved.
Step three: after the quartz capillary column to be coated is inserted into the sectional coating device, the solution of the sufficiently dissolved stationary phase is pressed into the quartz capillary column under the preset pressure, and two ends of the quartz capillary column are sealed.
Step four: the inner surface of the quartz capillary column is fully adhered with the high molecular coating, the distance between two adjusting plates of the sectional coating device is adjusted to be the same as the preset distance, the coating temperature and the coating time of the sectional coating device are set, and high-temperature coating is carried out.
Step five: after the high-temperature coating is finished, the quartz capillary column is washed by alkanes to remove the high-molecular stationary phase which is not heated by the high-temperature coating.
Step six: and aging for a preset time, and then taking down the treated quartz capillary column.
Further, the third step further comprises the step of leading out the stationary phase solution in the quartz capillary column after being sealed is attached for 24 hours.
The specific embodiment is as follows:
1. cutting a quartz capillary column with a certain length (generally 1-3 m, and inner diameter of 0.25-0.53 mm), cleaning the inner surface with alkane reagent, and controlling the cleaning pressure at 0.1-0.3MPa according to the inner diameter.
2. Dissolving the needed high molecular stationary phase with alkane reagent, controlling the dissolving concentration between 0.1mg and 0.25mg/mL according to the coating thickness, and using after fully dissolving.
3. Pressing the fully dissolved stationary phase into a quartz capillary column under certain pressure, and fully adhering for about 24 hours;
4. the quartz capillary column with the inner surface sufficiently adhered with the high molecular coating was inserted into a special coating apparatus to perform high temperature coating for 24 hours.
5. The quartz capillary column after high-temperature coating is washed to remove the high-molecular fixed phase which is not heated by high-temperature heating by using alkanes.
6. Aging was carried out for 24 hours.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A sectional coating device for the inner surface of a quartz capillary column comprises an adjustable heating box; the method is characterized in that: the adjustable heating box is provided with two adjusting plates capable of moving left and right; a heating pipe is arranged between the adjusting plates which move left and right; a cavity between the left and right adjusting plates forms a closed heating space, and a section to be heated of the quartz capillary column to be coated is suspended in the heating space; through holes capable of penetrating through a quartz capillary column to be coated are formed in the side wall of the adjusting heating box and the corresponding positions of the adjusting plate which moves left and right; an ultrasonic ranging unit for measuring the distance between the adjusting plates moving left and right is arranged between the adjusting plates moving left and right; also includes a control unit; the control unit comprises a singlechip, a temperature control circuit and a clock circuit; the temperature control circuit, the clock circuit and the ultrasonic ranging unit are all connected with the single chip microcomputer, and heating temperature control, heating time control and distance control between the adjusting plates of the heating space are achieved respectively.
2. The device of claim 1, wherein the inner surface of the quartz capillary column is coated by a step comprising: the adjusting plate moving left and right is driven to move left and right by a servo motor arranged outside the adjustable mounting box; an output shaft of the servo motor is connected with the screw rod to drive the screw rod to move; the screw rod drives the adjusting plate to move left and right; the motor control circuit is connected with the single chip microcomputer to realize the control of the motor.
3. The device of claim 1, wherein the inner surface of the quartz capillary column is coated by a step comprising: a temperature sensor is arranged in the closed heating space; the temperature sensor transmits the acquired information to the singlechip.
4. The device of claim 1, wherein the inner surface of the quartz capillary column is coated by a step comprising: also comprises a liquid device and a liquid pump; the liquid in the liquid device is pumped into the inner cavity of the quartz capillary column to be coated by a liquid pump; and the control circuit of the liquid pump is connected with the singlechip.
5. A sectional coating method for an inner surface of a quartz capillary column using the apparatus for sectional coating of an inner surface of a quartz capillary column according to any one of claims 1 to 4, characterized in that: the method comprises the following steps:
the method comprises the following steps: cleaning the inner surface of a quartz capillary column to be coated with an alkane reagent at the cleaning pressure of 0.1-0.3 MPa;
step two: dissolving the polymer stationary phase to be coated by an alkane reagent machine, wherein the dissolving concentration is 0.1-0.25 mg/mL, and the polymer stationary phase is used after being fully dissolved;
step three: after the quartz capillary column to be coated is inserted into the sectional coating device, the solution of the fully dissolved stationary phase is pressed into the quartz capillary column under the preset pressure, and two ends of the quartz capillary column are sealed;
step four: the inner surface of the quartz capillary column is fully adhered with the high molecular coating, the distance between two adjusting plates of the sectional coating device is adjusted to be the same as the preset distance, the coating temperature and the coating time of the sectional coating device are set, and high-temperature coating is carried out;
step five: after the high-temperature coating is finished, washing the quartz capillary column by alkanes to remove the high-molecular stationary phase which is not heated at the high temperature;
step six: and aging for a preset time, and then taking down the treated quartz capillary column.
6. The method of staged coating of an inner surface of a quartz capillary column according to claim 5, wherein: and step three, the quartz capillary column after being sealed is attached for 24 hours, and then the stationary phase solution in the quartz capillary column is led out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110685067.3A CN113264688A (en) | 2021-06-21 | 2021-06-21 | Sectional coating device and method for inner surface of quartz capillary column |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110685067.3A CN113264688A (en) | 2021-06-21 | 2021-06-21 | Sectional coating device and method for inner surface of quartz capillary column |
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| CN113264688A true CN113264688A (en) | 2021-08-17 |
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| CN202110685067.3A Pending CN113264688A (en) | 2021-06-21 | 2021-06-21 | Sectional coating device and method for inner surface of quartz capillary column |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082079A1 (en) * | 1981-12-14 | 1983-06-22 | The Dow Chemical Company | Process for etching and deactivating glass capillaries for chromatography |
| US4459173A (en) * | 1981-12-14 | 1984-07-10 | The Dow Chemical Company | Process for etching glass capillaries for chromatography |
| CN1106139A (en) * | 1994-05-12 | 1995-08-02 | 中国石化扬子石油化工公司 | Capillary chromatographic column filled with aluminum trioxide and its preparation method |
| WO2003054602A1 (en) * | 2001-12-20 | 2003-07-03 | 3M Innovative Properties Company | Sectionally photosensitive optical waveguides |
| CN1876586A (en) * | 2005-06-09 | 2006-12-13 | 李德建 | Production method of flexible quartz glass capillary for chromatography and special lower coating cup |
| WO2011017638A2 (en) * | 2009-08-07 | 2011-02-10 | Fas Holdings Group, Llc. | Segmented or selected-area coating |
| CN102512849A (en) * | 2011-12-31 | 2012-06-27 | 郑州大学 | Preparation method of capillary packed column |
-
2021
- 2021-06-21 CN CN202110685067.3A patent/CN113264688A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0082079A1 (en) * | 1981-12-14 | 1983-06-22 | The Dow Chemical Company | Process for etching and deactivating glass capillaries for chromatography |
| US4459173A (en) * | 1981-12-14 | 1984-07-10 | The Dow Chemical Company | Process for etching glass capillaries for chromatography |
| CN1106139A (en) * | 1994-05-12 | 1995-08-02 | 中国石化扬子石油化工公司 | Capillary chromatographic column filled with aluminum trioxide and its preparation method |
| WO2003054602A1 (en) * | 2001-12-20 | 2003-07-03 | 3M Innovative Properties Company | Sectionally photosensitive optical waveguides |
| CN1876586A (en) * | 2005-06-09 | 2006-12-13 | 李德建 | Production method of flexible quartz glass capillary for chromatography and special lower coating cup |
| WO2011017638A2 (en) * | 2009-08-07 | 2011-02-10 | Fas Holdings Group, Llc. | Segmented or selected-area coating |
| CN102512849A (en) * | 2011-12-31 | 2012-06-27 | 郑州大学 | Preparation method of capillary packed column |
Non-Patent Citations (1)
| Title |
|---|
| 万宏等: "超动态法快速制备毛细管色谱柱研究" * |
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Application publication date: 20210817 |
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