CN102107132A - Rectifying photochlorination device - Google Patents
Rectifying photochlorination device Download PDFInfo
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- CN102107132A CN102107132A CN200910260296XA CN200910260296A CN102107132A CN 102107132 A CN102107132 A CN 102107132A CN 200910260296X A CN200910260296X A CN 200910260296XA CN 200910260296 A CN200910260296 A CN 200910260296A CN 102107132 A CN102107132 A CN 102107132A
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Abstract
The invention discloses a rectifying photochlorination device. The rectifying photochlorination device mainly comprises a distilling still, a rectifying tower column, a rectifying tower head and a light source; chlorine, an inert gas and a liquid material enter the distilling still from a gas inlet and a liquid inlet of the distilling still, and a liquid product and a tail gas flow out from the outlet of the tower head so as to realize continuous production; the tower column and the tower head are made of quartz glass; the light source is arranged on the outer side of the tower column so as to be maintained conveniently; and the rectifying tower head is provided with a condenser and an electromagnetic valve, and switching of the rectifying tower between two states of full backflow and product taking is controlled through the electromagnetic valve, so the residence time of the liquid material is guaranteed and an aim of control of the product quality can be fulfilled. The device is used for producing high-purity silicon tetrachloride, can control the material to perform dynamic photo-chemical reaction under the condition of coexisting of the gas phase and the liquid phase, improve the photo-chemical efficiency and realize continuous production by controlling the in and out speeds of the raw materials and the products, and can save the production time and control the full backflow time simultaneously; and in the combination of the online sampling function, the products cannot be taken until the quality of the material is qualified.
Description
Technical field
The present invention relates to a kind of photochlorination apparatus, particularly rectifying formula photochlorination apparatus.
Background technology
Existing photochlorination apparatus roughly can be divided into three kinds, first kind is still formula photochlorination apparatus, built-in light-source is in still, for fast reaction speed, in the still reaction device that has agitator has been installed, this structure is having relatively high expectations to agitator often, the use that also has the pattern of outer circulation, reaction liquid is guided in the external circulating device, but is only depended on self power to be difficult to realize circulation, if adopt the pump circulation, so to the requirement of pump again than higher, in addition, also there is following problem in still formula photochlorination apparatus: dirt is often arranged on the lampshade of built-in light source, optical chlorinating reaction efficient is reduced, and safeguard relatively difficulty; Reaction heat is difficult to discharge, and causes side reaction to increase; Second kind of photochlorination apparatus is tower photochlorination apparatus, they adopt steel shell mostly, resistant materials such as liner tetrafluoro, light source is external, and in liquid material flowed into tower from cat head, chlorine entered in the tower at the bottom of by tower, gas-liquid two-phase contacts on column plate or baffle plate, make material generation optical chlorinating reaction by outer heater of tower and light source, the too small problem of the reaction unit ubiquity time of staying of this structure, photochemical reaction is insufficient; The third photochlorination apparatus is the tubular type photochlorination apparatus, and this device is equivalent to tower photochlorination apparatus horizontal positioned, though the time of staying increases to some extent, but controls than difficult for the flow regime of material.And, more than three kinds of photochlorination apparatus all have following problem: 1, material can only be that single-phase form exists; 2, be intermittent reaction, can not realize continuous production; 3, product quality can not On-line Control.
Summary of the invention
The objective of the invention is in order to solve the deficiency of above-mentioned technology, quartz glass system rectifying tower body is combined with photo-chlorination device, realize effects such as material full contact, the time of staying are controlled, On-line Product sampling, production continuously, two phase reaction, had the effect of rectification and purification simultaneously concurrently.
In order to achieve the above object, the present invention is by the following technical solutions:
Light chlorination rectifying column comprises: distillation still, king-post, tower head and light source, the rectifying king-post outside is equipped with light source, inert gas air inlet, chlorine air inlet, liquid inlet and higher boiling outlet are arranged on the distillation still), tower head is installed the magnetic valve 20 of the outflow of control gas-liquid.
Mainly comprise distillation still, rectifying tower body and light source, be connected with chlorine inlet, inert gas entrance and liquid material inlet on the distillation still, wherein, the chlorine inlet leads at the bottom of the still.Gas and liquid are controlled flow velocity by flowmeter.The distillation still heating part is made up of electrically heated rod, conduction oil and distillation still chuck, heating rod is earlier with the heat-conducting oil heating in the distillation still chuck, heat conduction by conduction oil makes temperature in the kettle raise, in the conduction oil and in the still temperature sensing device is housed respectively, is used for measuring and controlling oily gentle still temperature.Pressure-display device also is housed on the tower still, is used for the pressure of monitoring system.What link to each other with the tower still is the rectifying king-post, adopt the plate distillation column king-post, the material of king-post is a quartz glass, light source is installed in the outside, middle part at king-post, light source is a high-voltage ultraviolet mercury lamp, and lampshade is installed in the light source outside, avoids light that human body is damaged, adjustable fan is installed in the lampshade below, adjusts temperature in the lampshade by adjusting rotation speed of the fan.Rectifying king-post top is connected with distillation tower head, tower head is equipped with condenser, condenser comprises coiled structure in the tower head and jacket structured, guaranteed the condensation effect of tower head, temperature sensing device all is housed on king-post and the tower head measures temperature, simultaneously, magnetic valve is housed on the tower head, can control system in infinite reflux with get between the product and change, and can control the speed of getting product by reflux ratio, realized the purpose of controllable product quality, electromagnetic valve outlet connects a condenser pipe, and product is further cooled off, the condenser pipe end connects gas-liquid allotter, the gas piping of gas-liquid allotter is connected with the tail gas absorption system, can control system operate under negative pressure by this pipeline, and its liquid line is connected with online sample tap with the product bottle.The higher boiling that has bottom at the tower still exports.
Advantage of the present invention is: be used to produce highly purified silicon tetrachloride, obvious for the main hydrogen containing foreign trichlorosilane effect of removing in the silicon tetrachloride, the content of trichlorosilane is reduced to below the 1ppm.
Description of drawings
Fig. 1 is an overall construction drawing of the present invention.
Fig. 2 is the schematic diagram of light source among the present invention.
Fig. 3 is the schematic diagram of magnetic valve among the present invention.
Number in the figure is described as follows: the 1-distillation still; The 2-light source; 3 king-posts; The 4-tower head; 5-inert gas air inlet; 6-chlorine air inlet; The 7-fan; The 8-lampshade; 9,10,13 is temperature sensing device; The 11-cooling water inlet; The 12-coolant outlet; 14-liquid material inlet; The 15-pressure display unit; The 16-products export; The 17-gas-liquid allotter; The outlet of 18-tail gas; The 19-condenser pipe; The 20-magnetic valve; The 21-heating rod; The outlet of 22-higher boiling; The 23-air vent; The 24-magnetic pendulum; The 25-rotating shaft; The 26-liquid sealing pipe; The 27-electromagnet.
The specific embodiment
The present invention is further described in conjunction with example below by accompanying drawing.
Structure of the present invention as shown in Figure 1, comprise distillation still, king-post, tower head and light source, inert gas entrance 5, chlorine inlet 6 and liquid material inlet 14 are arranged on the distillation still, distillation still is by heating rod 21 and pass through heat-conducting oil heating, the distillation still top is connected to be king-post, the king-post top is connected to be tower head, form is a plate distillation column, in tower head, king-post and the distillation still still temperature sensing device is arranged all, pressure-display device 15 is arranged on the tower still, light source is installed in the king-post outside, and the tower head outlet is connected to magnetic valve 20, and liquid outlet 22 is arranged at tower still bottom.
By liquid material inlet 14 silicon tetrachloride is pressed in the still; feed a certain amount of inert gas as protective gas; be warming up to the material infinite reflux; feed chlorine; and open light source 2 simultaneously, under illumination condition, after infinite reflux a period of time, detect by products export 16 samplings; open magnetic valve 20 after qualified, regulate reflux ratio and get product.Be pressed into liquid charging stock by liquid material charging aperture 14 in distillation still 1 simultaneously, flow velocity is realized producing continuously with to get product speed identical.
Claims (7)
1. rectifying formula photochemical reaction device, it is characterized in that: it comprises: distillation still (1), king-post (3), tower head (4) and light source (2), rectifying king-post (3) outside is equipped with light source (2), inert gas air inlet (5), chlorine air inlet (6), liquid inlet (14) and higher boiling outlet (22) are arranged on the distillation still, and tower head is installed the magnetic valve (20) of the outflow of control gas-liquid.
2. rectifying formula photochemical reaction device according to claim 1, it is characterized in that: described king-post and tower head adopting quartz glass are made, and are the multi-deck screen plate structure in the king-post.
3. rectifying formula photochemical reaction device according to claim 1 and 2, it is characterized in that material is heated by conduction oil in the chuck in the described distillation still, insert heating rod (21) in the conduction oil, temperature sensing device (13) is housed in the tower still, the distillation still top is equipped with pressure-display device (15).
4. rectifying formula photochemical reaction device according to claim 1 and 2, it is characterized in that described light source (2) is a high-voltage ultraviolet mercury lamp, light source has lampshade (8) outward, lampshade (8) upper and lower side all has air vent (23), the lower port place is equipped with controlled fan (7), temperature sensing device (9) is installed between king-post (3) and the light source (2), is close to the king-post outer wall.
5. according to claim 1 and 2 described rectifying formula photochemical reaction devices, it is characterized in that tower head (4) is equipped with temperature sensing device (10), tower head has condenser on (4), and condenser is made up of the chuck and the upper port (12) (outlet) in lower port (11) (inlet), tower head inner coil pipe, the tower head outside.
6. rectifying formula photochemical reaction device according to claim 5 is characterized in that tower head (4) liquid outlet is connected with magnetic valve (20), and magnetic valve (20) outlet is connected with condenser pipe (19), and the end of condenser pipe (19) connects gas-liquid allotter (17).
7. rectifying formula photochemical reaction device according to claim 6 is characterized in that the liquid phase outlet (16) of gas-liquid allotter (17) connects product bottle and online sample connection, and gaseous phase outlet (18) connects device for absorbing tail gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910260296XA CN102107132A (en) | 2009-12-28 | 2009-12-28 | Rectifying photochlorination device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910260296XA CN102107132A (en) | 2009-12-28 | 2009-12-28 | Rectifying photochlorination device |
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| CN102107132A true CN102107132A (en) | 2011-06-29 |
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| CN200910260296XA Pending CN102107132A (en) | 2009-12-28 | 2009-12-28 | Rectifying photochlorination device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895932A (en) * | 2012-10-17 | 2013-01-30 | 联化科技股份有限公司 | Device for photo-catalytic bromination reaction |
| CN103143185A (en) * | 2013-03-21 | 2013-06-12 | 山东天一化学股份有限公司 | Diphenylethane rectifying device |
| CN104623967A (en) * | 2015-02-06 | 2015-05-20 | 北京凯德石英有限公司 | Primary filtering device, manufacturing method of primary filtering device and quartz glass purifying device |
| CN108129255A (en) * | 2017-12-14 | 2018-06-08 | 四川北方红光特种化工有限公司 | A kind of method and device of ortho-chlorotolu'ene synthesis o-chlorotrichlorotoluene |
| CN109336759A (en) * | 2018-12-03 | 2019-02-15 | 山东民基化工有限公司 | Continuously prepare the method and device thereof of chloro-pivalyl chloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4372834A (en) * | 1981-06-19 | 1983-02-08 | Bell Telephone Laboratories, Incorporated | Purification process for compounds useful in optical fiber manufacture |
| CN201245444Y (en) * | 2008-07-04 | 2009-05-27 | 湖北菲利华石英玻璃股份有限公司 | Quartz glass fractionating tower |
| CN201684601U (en) * | 2009-12-28 | 2010-12-29 | 北京有色金属研究总院 | Rectifying type photochlorination reaction unit |
-
2009
- 2009-12-28 CN CN200910260296XA patent/CN102107132A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4372834A (en) * | 1981-06-19 | 1983-02-08 | Bell Telephone Laboratories, Incorporated | Purification process for compounds useful in optical fiber manufacture |
| CN201245444Y (en) * | 2008-07-04 | 2009-05-27 | 湖北菲利华石英玻璃股份有限公司 | Quartz glass fractionating tower |
| CN201684601U (en) * | 2009-12-28 | 2010-12-29 | 北京有色金属研究总院 | Rectifying type photochlorination reaction unit |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895932A (en) * | 2012-10-17 | 2013-01-30 | 联化科技股份有限公司 | Device for photo-catalytic bromination reaction |
| CN103143185A (en) * | 2013-03-21 | 2013-06-12 | 山东天一化学股份有限公司 | Diphenylethane rectifying device |
| CN104623967A (en) * | 2015-02-06 | 2015-05-20 | 北京凯德石英有限公司 | Primary filtering device, manufacturing method of primary filtering device and quartz glass purifying device |
| CN108129255A (en) * | 2017-12-14 | 2018-06-08 | 四川北方红光特种化工有限公司 | A kind of method and device of ortho-chlorotolu'ene synthesis o-chlorotrichlorotoluene |
| CN109336759A (en) * | 2018-12-03 | 2019-02-15 | 山东民基化工有限公司 | Continuously prepare the method and device thereof of chloro-pivalyl chloride |
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Free format text: FORMER OWNER: BEIJING GUOJING INFRARED OPTICAL TECHNOLOGY CO., LTD. Effective date: 20130805 Owner name: BEIJING GUOJING INFRARED OPTICAL TECHNOLOGY CO., L Free format text: FORMER OWNER: BEIJING CENTRAL INST.OF THE NONFERROUS METAL Effective date: 20130805 |
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Effective date of registration: 20130805 Address after: 100088, 2, Xinjie street, Beijing Applicant after: Beijing Guojing Infrared Optical Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Applicant before: General Research Institute for Nonferrous Metals Applicant before: Beijing Guojing Infrared Optical Technology Co., Ltd. |
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