CN204649473U - A kind of segmented cleaning formula sampling system of producing for methyl chlorosilane - Google Patents
A kind of segmented cleaning formula sampling system of producing for methyl chlorosilane Download PDFInfo
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- CN204649473U CN204649473U CN201520217546.2U CN201520217546U CN204649473U CN 204649473 U CN204649473 U CN 204649473U CN 201520217546 U CN201520217546 U CN 201520217546U CN 204649473 U CN204649473 U CN 204649473U
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Abstract
The utility model discloses a kind of segmented cleaning formula sampling system of producing for methyl chlorosilane, the process pipeline that methyl chlorosilane is produced is provided with the back flow of sample point of at least two sampled points and correspondence, is provided with cycles samples pipeline between each sampled point with corresponding back flow of sample point; Each sample circulation line is equipped with sampling slip, and all sampling slips are by respective transfer valve group access sampling house steward, and this sampling house steward is communicated with the injection port of analytical instrument by preheating device, between sampling house steward and preheating device, be provided with cleaning interface; Described sampling system also comprises waste liquid house steward, and described transfer valve group comprises two T-valve; Every bar sample circulation line is provided with purging interface, is provided with the discharging tube being connected to described waste liquid house steward in check valve downstream.The process pipeline that the utility model is produced at methyl chlorosilane arranges multiple sampled point and carries out real-time sampling, relevant sample lines is carried out to the cleaning of different modes, maintain the normal operation of sampling system.
Description
Technical field
The utility model relates to organosilicon production field, is specifically related to a kind of segmented cleaning formula sampling system of producing for methyl chlorosilane.
Background technology
Methyl chlorosilane is the general designation of direct synthesis product, and general molecular formula is (CH
3)
xh
ysiCl
4-x-yat present, industrial production methyl chlorosilane monomer mainly carries out high-temperature high-voltage reaction preparation, in this course of reaction by methyl chloride gas and silica flour in fluidized bed under copper catalyst effect, synthetic product reaches tens kinds, needs to carry out separation and purification in the use procedure of reality.
The purity requirement of methyl chlorosilane downstream product to methyl chlorosilane monomer is varied, such as, when preparing heat vulcanized silicone rubber, very high to the requirement of key starting material dimethyldichlorosilane purity, the boiling point of dimethyldichlorosilane (boiling point 70.5 DEG C) and methyl trichlorosilane (boiling point 66.4 DEG C) and the hydrogeneous dichlorosilane of ethyl (boiling point 75.5 DEG C) all closely, three is not easy to be separated, and methyl trichlorosilane and the hydrogeneous dichlorosilane of ethyl belong to three-functionality-degree impurity, there is serious harm to the performance of silicon rubber.
In prior art, the technological process of production of methyl chlorosilane monomer is divided into fluidized bed reaction system, washing, purifying just point recovery system and distillation system three bulk, the main technological process of production as shown in Figure 1, comprise the fluidized reactor, purifying dust-removing device, the first rectification column, Second distillation column, relay tank, the 3rd rectification column, the 4th rectification column, the 5th rectification column that set gradually along material moving direction, and for the liquid waste tank of batch process accident waste material.The entrance of rectification column at different levels is equipped with corresponding feeder pump.
Wherein, fluidized reactor, namely large-scale fluidized bed, in fluidized reactor, methyl chloride gas and silica flour carry out high-temperature high-voltage reaction under copper catalyst effect, obtain methyl chlorosilane monomer.
Purifying dust-removing device comprises the three-stage cyclone separator and cleaning dust tower that connect successively, wherein, front two stage cyclone separation vessel is separated the solid that obtains and reclaims to enter in fluidized reactor and again participate in reaction, and the solid that afterbody cyclone separator and cleaning dust tower obtain is as waste discharge.
Cleaning dust tower is provided with overhead condenser, and the liquid phase of overhead condenser enters Second distillation column, and the gas phase of overhead condenser enters the first rectification column.
The material flowed out by the first rectifier bottoms enters Second distillation column, and enter relay tank by the material flowed out bottom Second distillation column, add other monomer and be in harmonious proportion in relay tank, the potpourri after mediation enters in the 3rd rectification column.
The material that 3rd rectification column (i.e. de-low tower) bottom is flowed out enters the 4th rectification column, and the 3rd rectification column top obtains low-boiling-point substance; The material that 4th rectification column (i.e. de-high tower) top is flowed out enters the 5th rectification column, and the 4th rectifier bottoms obtains high-boiling components.The top of the 5th rectification column obtains methyl trichlorosilane, and the bottom of the 5th rectification column obtains dimethyldichlorosilane.
Because the technological process of production of methyl chlorosilane monomer is very complicated, in order to optimize the technique of production better, need to carry out sample analysis to the links in production run, obtain accurate physical data, according to the result of Physical Property Analysis, processing parameter is adjusted, promotes quality and the output capacity of product.
Utility model content
The utility model provides a kind of segmented cleaning formula sampling system of producing for methyl chlorosilane, the process pipeline that methyl chlorosilane is produced arranges multiple sampled point and carries out real-time sampling, and can relevant sample lines be cleaned, maintain the normal operation of sampling system.
For the segmented cleaning formula sampling system that methyl chlorosilane is produced, the process pipeline that methyl chlorosilane is produced is provided with the back flow of sample point of at least two sampled points and correspondence, is provided with cycles samples pipeline between each sampled point with corresponding back flow of sample point; Each sample circulation line is equipped with sampling slip, and all sampling slips are by respective transfer valve group access sampling house steward, and this sampling house steward is communicated with the injection port of analytical instrument by preheating device, between sampling house steward and preheating device, be provided with cleaning interface;
Described sampling system also comprises waste liquid house steward, and described transfer valve group comprises two T-valve, wherein:
Two ports of upstream three-way valve are connected in sampling slip, and the 3rd port is connected to waste liquid house steward;
Two ports of downstream T-valve are connected in sampling house steward, and the 3rd port is connected to sampling slip;
Every bar sample circulation line is provided with prefilter, fine filter, flowmeter and non-return valve successively, described sampling slip is connected between fine filter and flowmeter, between prefilter and fine filter, be provided with purging interface, be provided with the discharging tube being connected to described waste liquid house steward in check valve downstream.
Quantity and the position of the back flow of sample point of sampled point and correspondence can be selected according to needs, every bar sample circulation line is equivalent in existing process equipment, set up a loop, in normal production run, material continuous flow in cycles samples pipeline, when needing sampling, by controlling the transfer valve group on sampling slip, sampling slip is communicated with sampling house steward, thus material is entered in analytical instrument via sampling slip and sampling house steward.
When not sampling, respectively by cleaning interface and the cleaning medium purging interface introducing outside, segmented cleaning is carried out to the associated pipe of sampling system.
Described cleaning orifice has cleaning surge chamber, and this cleaning surge chamber is respectively equipped with cleaning solvent supply pipe, compressed nitrogen supply pipe and blow-down pipe.
Cleaning solvent is driven (to adopt acetone by compressed nitrogen, pressurized air drives cleaning solvent can adopt the mode of injection) carry out the flushing of pipeline, by controlling the valve in respective line, cleaning solvent can be controlled and do not enter analytical instrument, but along tube runs in liquid header, complete the cleaning to pipeline on the way.
Described purging orifice has compressed air supply system, compressed air supply system carries pressurized air by purging interface in corresponding pipeline, the each T-valve controlled in transfer valve group enables pressurized air be circulated to discharging tube, and being circulated to liquid header further by discharging tube, the refuse in the pipeline that pressurized air is flowed through is purged totally.
Prefilter and fine filter are used for carrying out filter operation to material, and cleaning of protection channel interior, flowmeter is for measuring the mass flow in cycles samples pipeline, and non-return valve is used for preventing Flow of Goods and Materials direction from taking a turn for the worse.
Every bar sample circulation line is equipped with control main valve with between corresponding sampled point and back flow of sample point.If a certain sampled point does not need to sample, or when needing to keep in repair, can turn off corresponding cycles samples pipeline by controlling main valve.
All transfer valve groups are arranged in a sample pretreatment switch board, described discharging tube is provided with manual sampling slip, and manual sampling slip is positioned at the outside of sample pretreatment switch board, when sampling slip breaks down, can manually sampling slip, carry out sample collection.
Described prefilter is two groups of line strainers in parallel.If when wherein one group of line strainer breaks down or needs maintenance and change, other one group of line strainer can be used.
In sampling slip, be provided with the isolation valve between cycles samples pipeline and described transfer valve group, in fine filter upstream, check valve downstream and isolation valve downstream be respectively equipped with pressure gauge.Isolation valve is for cutting off cycles samples pipeline and being communicated with between sampling slip.
Described sampling house steward is provided with two threeway sampling switching valves, and two ports of each threeway sampling switching valve are connected in sampling house steward;
The injection port of the 3rd port linking parsing instrument of the threeway sampling switching valve of upstream;
The outlet of the 3rd port linking parsing instrument of the threeway sampling switching valve in downstream.
Two threeway sampling switching valves can control to sample the sample flowed in house steward and not enter analytical instrument, but pass back in a certain production equipment, such as, pass back into the discharging opening of the overhead condenser of cleaning dust tower.
Upstream in the utility model or downstream are that material moves to downstream by upstream for Flow of Goods and Materials direction.
The utility model is used for the segmented cleaning formula sampling system that methyl chlorosilane is produced, the process pipeline that methyl chlorosilane is produced arranges multiple sampled point and carries out real-time sampling, and the character feature of the material flowed in foundation pipeline, relevant sample lines is carried out to the cleaning of different modes, maintain the normal operation of sampling system.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of methyl chlorosilane production run in prior art;
Fig. 2 is the schematic diagram of the segmented cleaning formula sampling system that the utility model is produced for methyl chlorosilane;
Fig. 3 is the E portion enlarged drawing in Fig. 2.
Embodiment
Below in conjunction with accompanying drawing, segmented cleaning formula sampling system the utility model being used for methyl chlorosilane production is described in detail.
As shown in Figure 2, for the segmented cleaning formula sampling system that methyl chlorosilane is produced, the process pipeline that methyl chlorosilane is produced arranges four sampled points, is respectively sampled point A, sampled point B, sampled point C, sampled point D; Each sampled point correspondence arranges a back flow of sample point, is respectively back flow of sample point A, back flow of sample point B, back flow of sample point C, back flow of sample point D, is provided with cycles samples pipeline between each sampled point with corresponding back flow of sample point.
Every bar sample circulation line is provided with a corresponding sampling slip, and all sampling slips are by respective transfer valve group access sampling house steward, and sampling house steward is communicated with the injection port of analytical instrument.
Analytical instrument can adopt prior art, and the physical parameter obtained as required selects suitable instrument to analyze.
Every bar sample circulation line is equivalent in existing process equipment, set up a loop, in normal production run, material continuous flow in cycles samples pipeline, when needing sampling, by controlling the transfer valve group on sampling slip, sampling slip is communicated with sampling house steward, thus material is entered in analytical instrument via sampling slip and sampling house steward.
The structure of each sample circulation line and corresponding sampling slip is substantially identical, be described in detail for the cycles samples pipeline formed between sampled point D and back flow of sample point D and sampling slip below, as Fig. 2, shown in Fig. 3, every bar sample circulation line is provided with prefilter successively, fine filter 2, flowmeter 3, non-return valve 4, and pressure gauge, sampling slip is connected between fine filter 2 and flowmeter 3, be provided with between cycles samples pipeline and corresponding sampled point D and control main valve 16, be equipped with between cycles samples pipeline with corresponding back flow of sample point D and control main valve 17.
Prefilter is two groups of line strainers 1 in parallel, is respectively equipped with valve at the upstream and downstream of each line strainer 1.
In sampling slip, be provided with the isolation valve 5 between cycles samples pipeline and transfer valve group, be respectively equipped with pressure gauge in the downstream of the upstream of fine filter 2 and isolation valve 5.
As shown in Figure 2, the members of sampling system is arranged in a sample pretreatment switch board G, and pipeline represents with square through the node of sample pretreatment switch board G.
It is inner that the pressure gauge in fine filter 2, flowmeter 3, non-return valve 4, isolation valve 5, fine filter 2 upstream and isolation valve 5 downstream is all positioned at sample pretreatment switch board G, the cycles samples pipeline being in sample pretreatment switch board G both sides is respectively equipped with valve, inside and outside sample pretreatment switch board G, conducting and the disconnection of cycles samples pipeline can be carried out respectively.
The emergency bypass in parallel with fine filter 2, flowmeter 3, non-return valve 4 is provided with in sample pretreatment switch board G, when needing to overhaul fine filter 2, flowmeter 3, non-return valve 4 or change, enable emergency bypass, material is continuous flow in emergency bypass, to normally not impacting of whole production run.
Between prefilter and fine filter 2, be provided with purging interface, purging interface has compressed air supply system by pipeline connection, and pipeline is provided with valve.
Compressed air supply system carries pressurized air by purging interface in corresponding pipeline, the each T-valve controlled in transfer valve group enables pressurized air be circulated to discharging tube, and being circulated to liquid header further by discharging tube, the refuse in the pipeline that pressurized air is flowed through is purged totally.
Sampling system also comprises waste liquid house steward 6, is provided with the discharging tube 7 being connected to waste liquid house steward 6 in non-return valve 4 downstream, and discharging tube 7 is provided with manual sampling slip 8, and discharging tube 7 and manual sampling slip 8 are respectively equipped with valve.
Transfer valve group on sampling slip comprises two T-valve, and be respectively the T-valve 91 being in upstream and the T-valve 92 being in downstream, port a and the port b of T-valve 91 are connected in sampling slip, and port c is connected to waste liquid house steward 6; The port f of T-valve 92 and port e is connected in sampling house steward, and port d is connected to sampling slip.
On sampling slip, each T-valve of transfer valve group all connects and is controlled by the signal of timing circuit and flowmeter 3, and when flowmeter meets setting range, timing circuit controls transfer valve group and opens different sampling slips successively to sampling house steward in chronological order.
Sampling house steward is provided with two threeway sampling switching valves, is respectively threeway sampling switching valve 81 and threeway sampling switching valve 82, and two ports of threeway sampling switching valve 81 are connected in sampling house steward, the injection port of the 3rd port linking parsing instrument; Two ports of threeway sampling switching valve 82 are connected in sampling house steward, the outlet of the 3rd port linking parsing instrument.
Sampling house steward is communicated with the injection port of analytical instrument by preheating device 11, cleaning interface is provided with between sampling house steward and preheating device 11, cleaning orifice has cleaning surge chamber 12, cleaning surge chamber 12 is respectively equipped with cleaning solvent supply pipe 13 (cleaning solvent employing acetone), compressed nitrogen supply pipe 14 and blow-down pipe 15.
By controlling the valve in respective line, making cleaning solvent not enter analytical instrument, but along tube runs in liquid header, completing the cleaning to pipeline on the way.
Number and the position of the back flow of sample point of sampled point and correspondence can be selected as required, on the basis of the sampling system given by the utility model, pressure release can be set further, the pipeline such as overhaul reserve and back flow of sample, ensure the safe and stable operation of whole sampling system.
As shown in Figure 1 and Figure 2, four sampled points in present embodiment and the back flow of sample point of correspondence are respectively:
Sampled point A: the discharging opening of the overhead condenser of cleaning dust tower, material is herein about 80% crude monomer+20% chloromethanes;
Back flow of sample point A: liquid waste tank;
Sampled point B: discharging opening at the bottom of the tower of Second distillation column;
The entrance of the feeder pump of back flow of sample point B: the three rectification column;
The charging delivery side of pump of sampled point C: the three rectification column;
The entrance of the feeder pump of back flow of sample point C: the three rectification column;
The charging delivery side of pump of sampled point D: the five rectification column, material composition is herein about the methyl trichlorosilane of 80 ~ 90% and the potpourri of dimethyldichlorosilane, not containing trimethyl chlorosilane.
The entrance of the feeder pump of back flow of sample point D: the three rectification column.
The difference of the back flow of sample point position of foundation sampled point and correspondence, the structure of cycles samples pipeline and sampling slip is slightly different, such as, the temperature of the material that sampled point D gathers is higher, in the sampling slip that sampled point D is corresponding, arrange heat interchanger 18 lower the temperature, temperature of charge is met enter the requirement of analytical instrument.
When the sampling system adopting the utility model to provide is sampled, cycles samples pipeline to be sampled is specified successively according to time sequencing, and the mass flow detected in real time in each sample circulation line, when mass flow in current sample circulation line meets setting range and is designated, carry out material composition analysis by the sampling slip automatic sampling be connected with cycles samples pipeline to analytical instrument.
Claims (9)
1. a segmented cleaning formula sampling system of producing for methyl chlorosilane, it is characterized in that, the process pipeline that methyl chlorosilane is produced is provided with the back flow of sample point of at least two sampled points and correspondence, is provided with cycles samples pipeline between each sampled point with corresponding back flow of sample point; Each sample circulation line is equipped with sampling slip, and all sampling slips are by respective transfer valve group access sampling house steward, and this sampling house steward is communicated with the injection port of analytical instrument by preheating device, between sampling house steward and preheating device, be provided with cleaning interface;
Described sampling system also comprises waste liquid house steward, and described transfer valve group comprises two T-valve, wherein:
Two ports of upstream three-way valve are connected in sampling slip, and the 3rd port is connected to waste liquid house steward;
Two ports of downstream T-valve are connected in sampling house steward, and the 3rd port is connected to sampling slip;
Every bar sample circulation line is provided with prefilter, fine filter, flowmeter and non-return valve successively, described sampling slip is connected between fine filter and flowmeter, between prefilter and fine filter, be provided with purging interface, be provided with the discharging tube being connected to described waste liquid house steward in check valve downstream.
2., as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, every bar sample circulation line is equipped with control main valve with between corresponding sampled point and back flow of sample point.
3., as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, described cleaning orifice has cleaning surge chamber, and this cleaning surge chamber is respectively equipped with cleaning solvent supply pipe, compressed nitrogen supply pipe and blow-down pipe.
4., as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, described purging orifice has compressed air supply system.
5., as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, described discharging tube is provided with manual sampling slip.
6. as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, described prefilter is two groups of line strainers in parallel.
7. as claimed in claim 1 for the segmented cleaning formula sampling system of methyl chlorosilane production, it is characterized in that, in sampling slip, be provided with the isolation valve between cycles samples pipeline and described transfer valve group, in fine filter upstream, check valve downstream and isolation valve downstream be respectively equipped with pressure gauge.
8., as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, all transfer valve groups are arranged in a sample pretreatment switch board.
9. as claimed in claim 1 for the segmented cleaning formula sampling system that methyl chlorosilane is produced, it is characterized in that, described sampling house steward is provided with two threeway sampling switching valves, and two ports of each threeway sampling switching valve are connected in sampling house steward;
The injection port of the 3rd port linking parsing instrument of the threeway sampling switching valve of upstream;
The outlet of the 3rd port linking parsing instrument of the threeway sampling switching valve in downstream.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223254A (en) * | 2015-11-16 | 2016-01-06 | 云南华联锌铟股份有限公司 | A kind of sampling pre-service and multithread road switch PH measurement mechanism |
| CN111473185A (en) * | 2020-04-25 | 2020-07-31 | 重庆三联管道设备有限公司 | Cleaning method of process pipeline |
-
2015
- 2015-04-10 CN CN201520217546.2U patent/CN204649473U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223254A (en) * | 2015-11-16 | 2016-01-06 | 云南华联锌铟股份有限公司 | A kind of sampling pre-service and multithread road switch PH measurement mechanism |
| CN105223254B (en) * | 2015-11-16 | 2017-08-29 | 云南华联锌铟股份有限公司 | One kind sampling pretreatment and many streams switch PH measurement apparatus |
| CN111473185A (en) * | 2020-04-25 | 2020-07-31 | 重庆三联管道设备有限公司 | Cleaning method of process pipeline |
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