CN110433507B - Method for automatically discharging silane slurry slag according to solid content - Google Patents
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- 239000002893 slag Substances 0.000 title claims abstract description 131
- 239000007787 solid Substances 0.000 title claims abstract description 73
- 238000007599 discharging Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 35
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 32
- 238000001704 evaporation Methods 0.000 claims abstract description 49
- 230000008020 evaporation Effects 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 11
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- 230000005251 gamma ray Effects 0.000 claims description 5
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- 238000012544 monitoring process Methods 0.000 claims description 5
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- 239000010802 sludge Substances 0.000 claims description 4
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- 239000011261 inert gas Substances 0.000 claims description 2
- 238000009834 vaporization Methods 0.000 claims 2
- 230000008016 vaporization Effects 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
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- 238000004134 energy conservation Methods 0.000 abstract description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 17
- 239000005046 Chlorosilane Substances 0.000 description 14
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 14
- 238000011282 treatment Methods 0.000 description 14
- 239000013049 sediment Substances 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 239000011863 silicon-based powder Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910007161 Si(CH3)3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000003379 elimination reaction Methods 0.000 description 1
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- 230000008570 general process Effects 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for automatically discharging silane slurry slag according to solid content, which comprises the following steps: the material separated from heavy components in the washing tower enters an evaporation system, and the evaporation system is heatedEvaporating light components, discharging the slurry slag concentrated by the evaporation system to a slurry slag sending system, and discharging the slurry slag; wherein the discharge time interval of the slurry slag in the sending system is calculated according to a formula shown in a formula (I): t isn=Tn‑1+Tn‑1×(P0‑Pn‑1)/P0(I) In that respect The method for treating the silane slurry slag can effectively reduce the discharge amount, reduce the blocking times, save the production cost of organic silicon, meet the requirements of energy conservation and emission reduction, and is suitable for industrial large-scale popularization.
Description
Technical Field
The invention relates to the technical field of organic silicon, in particular to a method for discharging silane slurry slag in the organic silicon industry.
Background
The organic silicon is a novel chemical product with excellent performance and wide application, and can be widely applied to the living fields of textiles, automobiles, buildings, electronics, cosmetics and the like and the special fields of national defense and the like. A plurality of organic silicon products mainly come from a direct method monomer synthesis device, and the general process flow is as follows: liquid phase chlorosilane is gasified by a vaporizer after being metered, heated by a superheater and then enters a fluidized bed through a distribution plate, silicon powder and a catalyst are mixed and then enter the fluidized bed through a fluidized bed feeding port, the reaction is started by heating heat conduction oil, and after the reaction is normal, the reaction heat release is taken away by cold conduction oil. In order to maintain the fluidized bed level and reaction, silicon powder and catalyst are required to be supplemented continuously. Synthetic gas (which is reaction product silane, unreacted chloromethane, fine silicon powder and catalyst) enters a cyclone system through the top of a fluidized bed, the synthetic gas of the fluidized bed reactor carries fine powder, large-particle fine powder is captured through the cyclone separation system firstly, then heavy components in chlorosilane are further separated through a washing tower system, and the heavy components comprise the fine powder which is not captured by the cyclone system and high-boiling-point silane. And evaporating the heavy component by flash evaporation and other evaporation treatments to evaporate the light component, extracting partial silane, and commonly referring the rest part as silane slurry residue. The light component is mainly chlorosilane with a boiling point of less than 160 ℃ and Comprises (CH)3)3Si2(CH3)3Cl2,(CH3)3SiCH2Si(CH3)3Cl2,(CH3)3Si2(CH3)2Cl,(CH3)3Si2(CH3)Cl2,(CH3)3SiCH2Si(CH3)2Cl, and the like. The silane slurry slag is a solid-liquid mixture, and the main component of the silane slurry slag is high-boiling-point substances>160 ℃), fine silicon powder and fine catalysts (Cu, Zn, Sn, etc.), the main components of the high-boiling-point substances are high-boiling-point chlorosilane, and the high-boiling-point chlorosilane is easy to deliquesce when meeting air containing moisture, generates HCl, forms acid mist, has strong corrosiveness and irritation, is not only harmful to equipment (centrifuger, etc.) and operators, but also is easy to stick and block due to the fact that the chlorosilane hydrolyzes to generate colloid, and seriously influences production stability and operability. The liquid is high boiling point chlorosilane, and the solid is silicon powder and catalyst. The solid content range of the synthetic slurry slag discharge is 40-60%, chlorosilane waste is caused by low solid content discharge, and slag discharge blockage is caused by high solid content discharge.
In the prior art, the problem of harmless treatment of slurry slag is not effectively solved all the time, and a plurality of factories are simply buried or burned, so that the environment is greatly polluted. CN106623370A discloses a silane slurry residue treatment process and a system, which relate to the hydrolysis of chlorosilane and generate a large amount of hydrogen chloride gas, and although acid mist generated by hydrolysis is absorbed in the patent, the problems of equipment corrosion, potential safety hazard and environmental pollution are not effectively solved. CN104045059A discloses a silane slurry hydrolysis treatment process, which employs curing agents, such as carbonate and silicon dioxide, which do not react with slurry and can neutralize hydrochloric acid. However, although the discharge of hydrogen chloride generated during hydrolysis is reduced, the method causes the treatment cost of the silane slurry slag to be overhigh, and is not suitable for industrial popularization. CN102118605A discloses a silane slurry slag treatment process, which adopts lime water to treat silane slurry slag, and solves the problems of equipment corrosion, potential safety hazard elimination of operators and pollution caused by hydrogen chloride gas released by slurry slag when meeting water. However, the slurry slag after the lime water treatment cannot be utilized, and the solid content in the slurry slag becomes high after the treatment, so that the treatment difficulty of the slurry slag becomes high, the cost becomes high, and the economic benefit is low. CN106220666A, CN107501315A, both disclose an apparatus and a method for treating silane sludge. The evaporation system is used for concentrating the synthetic slurry slag in the prior art, an operator judges the temperature or the material level of the evaporation system, then the slurry slag is discharged to the slurry slag tank, the slurry slag tank is sent to the slurry slag hydrolysis device, and the slurry slag after the pipeline is connected is sent to the slurry slag hydrolysis system for hydrolysis. Hydrolyzing the pulp residue to generate black solid hydrolysate and oily acid water, wherein the black solid hydrolysate is hazardous waste. The slurry residue discharge amount is too much, so that more chlorosilane is discharged, the unit consumption of raw materials is increased, more sewage and black solid hydrolysate are generated, the environment is polluted, and the treatment cost is increased. The discharge amount of the slurry slag is too small, the slurry slag is easy to block an evaporation system, a sending system and pipelines thereof, chlorosilane is flammable liquid, and the synthesized slurry slag is discharged at high temperature, so that the safety risk is high. Therefore, how to discharge the slurry slag is crucial to organic silicon production enterprises in reducing solid waste and sewage generation, safe production and reducing consumption.
Disclosure of Invention
The invention aims to overcome the defects of discharging the slurry slag in the organic silicon production in the prior art, provides a method for discharging the slurry slag according to the solid content of the slurry slag, and can effectively reduce the discharge amount of the slurry slag, reduce pollution, ensure safe production and reduce cost by matching with a simple and quick solid content test mode. The discharge time interval is determined according to the solid content, and the silane slurry slag is automatically discharged, so that the slurry slag discharge is reduced, the raw material utilization rate is improved, the slurry slag treatment cost is reduced, and the blocking times are reduced.
The purpose of the invention is realized by the following technical scheme:
a method for automatically discharging silane slurry slag according to solid content comprises the following steps: the material separated from the heavy component by the washing tower enters an evaporation system, the evaporation system is heated to evaporate the light component, the slurry and slag concentrated by the evaporation system are discharged to a slurry and slag sending system, and then the slurry and slag are discharged; wherein the discharge time interval of the slurry slag in the sending system is calculated according to a formula shown in a formula (I):
Tn=Tn-1+Tn-1×(P0-Pn-1)/P0 (I)
wherein n is the number of times of discharging the slurry slag, n is more than or equal to 1, TnIs the slurry and slag discharge time interval, T, of the nth operationn-1Is the slurry and slag discharge time interval P of the n-1 th operation0Is the target set value of the solid content of the slurry slag, Pn-1Is the solid content of the slurry residue in the n-1 st operation. When n is 1, Tn-1Is T0,T0The initial discharge time interval of the slurry slag is set.
Target set value P of solid content of slurry slag030-60 (%), preferably 45-55 (%); and/or T0In the range of 3 to 8, more preferably 4 to 6 hours.
The evaporation system comprises an evaporation tank, a temperature monitoring system and a material level meter, wherein silane slurry slag is continuously discharged from the washing tower and enters the evaporation system through a feed valve, the evaporation system intermittently discharges materials to a sending system, the evaporation system is connected with the sending system through a discharging pipe and a pressure equalizing pipe, a pressure equalizing valve is installed on the pressure equalizing pipe, the pressure equalizing pipe is connected with a pressure charging pipeline provided with the pressure equalizing valve, the pressure equalizing valve is used for balancing the pressure of the evaporation system and the sending system, and the pressure charging valve is used for charging inert gas such as N2And the like.
The organosilicon material is continuously fed from the washing tower to an evaporation system, and the temperature of the evaporation system is 120-200 ℃, preferably 150-180 ℃ when the evaporation system works.
The transmitting system comprises a transmitting tank, a level meter and a densimeter, wherein the level meter and the densimeter preferably adopt a gamma-ray level meter integrating the level meter and the densimeter.
The discharge interval of the discharged slurry slag in the sending system is obtained by calculation according to the solid content of the slurry slag, wherein the calculation formula of the solid content is shown as the following formula (II):
the D1 discharge system measures the pulp density, the solid density in D2 pulp and the liquid density in D3 pulp; wherein the solid density is calculated by referring to the composition of the fine powder collected by the cyclone; the liquid density is obtained by calculating the liquid phase composition of the slurry residue or directly measuring the liquid phase density; the density of the slurry slag is measured by gamma ray.
The density D2 of the solid fine powder of the slurry residue is calculated according to the following formula (III):
where ρ is the density of the solid and A is the mass fraction of the solid. For example, when the solid in the slurry slag mainly comprises silicon powder and metallic copper, the density D2 of the solid in the slurry slag is calculated by the mass percent of silicon element in the silicon powder multiplied by the mass percent of silicon element in the fine powder and the mass percent of metallic copper multiplied by the mass percent of copper element in the fine powder; the density of D2 is generally 2200-3。
The slurry-residue liquid density D3 is generally tested at 160 ℃ and is 1000-1300kg/m3。
When the sending system works and is pressurized, the system pressure is 2-5bar, preferably 3-4 bar; at the end of the discharge, the system pressure is between 0.2 and 1.0bar, preferably between 0.3 and 0.7 bar.
In a preferred technical scheme of the invention, the method for automatically discharging the silane slurry slag according to the solid content comprises the following steps:
(1) the method comprises the initial step that after the monomer synthesis device is started to normally produce, a system for automatically discharging the slurry slag according to the solid content is started to be used, the automatic program automatically records the discharge time interval and the solid content of the slurry slag discharged by a sending tank, and the temperature of an evaporation system can reach 160 ℃;
(2) a waiting step, after the slurry slag is conveyed to a sending system, calculating the time interval of the slurry slag discharging according to a formula (I), and starting the slurry slag filling step when the timing time interval is reached;
(3) filling: opening a pressure equalizing valve of the evaporation system, waiting for 30-60s, starting timing of the next slurry slag discharge time interval, opening a blanking valve between the evaporation system and the sending system, conveying the material in the evaporation system to the sending system, closing the blanking valve when the material level of the sending tank reaches 70-100% of the set material level, waiting for 30-60s, recording the slurry slag density in the sending tank, and further calculating the solid content of the slurry slag;
4) a sending step: closing the pressure equalizing valve, opening a pressurizing valve of the evaporation system, pressurizing to 2-5bar, opening the discharging valve for discharging, waiting for 30-60s when the material level of the sending tank reaches 5-10% of the material level, closing the pressurizing valve, closing the discharging valve when the system pressure is reduced to 0.3-0.7bar, ending the sending program, continuing waiting for the next time of discharging time interval, timing, and repeating the step (2) -the step (4).
Compared with the prior art, the invention has the following beneficial effects:
firstly, the slurry slag discharging method of the invention is adopted to adjust the discharging interval time of the slurry slag according to the solid content change, thereby achieving the purpose of reducing the slurry slag discharging amount, not only increasing the utilization degree of upstream materials, but also reducing the treatment capacity of the slurry slag, greatly saving the production cost of organic silicon, and simultaneously meeting the requirements of China on energy conservation and emission reduction of factories.
The slurry and slag are sent by using the sending system, and the safe operation can be realized without dismounting the pipeline and accessories.
Setting up the densimeter in thick liquid sediment discharge system, can calculating through the material density in the monitoring system and obtain the solid content of thick liquid sediment, and then decide thick liquid sediment discharge time interval according to the value that the solid content of thick liquid sediment was contained for thick liquid sediment is stably discharged, and is accurate high-efficient, has avoided carrying out the defect that discharges the thick liquid sediment too much or too little that the manual experience operation that discharges caused according to material level or temperature in the past.
Fourthly, the slurry slag is automatically discharged, the workload of an operator is reduced, and the inaccuracy caused by the operator through judgment according to experience is also reduced.
And fifthly, the chlorosilane in the slurry slag is hydrolyzed to generate colloid which is easy to be sticky, and the accuracy of the solid content test result in the slurry slag is seriously influenced. The conventional method for measuring the solid content is not suitable for silane slurry slag generated in organic silicon production, and aiming at the problem that the solid content in the slurry slag is difficult to test, the invention provides a method for monitoring the material density in a system by adopting a densimeter to obtain the solid content of the slurry slag, so as to control the discharge time interval of the slurry slag.
Drawings
FIG. 1 is a schematic view of a silane sludge discharge system in the practice of the present invention.
Detailed Description
The method for discharging silane slurry slag according to the solid content of the invention is further explained in detail with reference to the following specific embodiments, the chlorosilane used in the examples is methyl chlorosilane, which is the most commonly used halosilane in organosilicon, but it should not be construed as limiting the scope of the invention, and for other halosilanes, the method for discharging silane slurry slag provided by the invention can achieve similar technical effects and can also solve the technical problems to be solved by the invention, and thus is also within the scope of the invention.
The schematic diagram of the silane slurry slag discharge system adopted in the embodiment of the invention is shown in figure 1, wherein the material enters the evaporation system through an evaporation system feed valve V1, the pressure is regulated through a pressure equalizing valve V4, and the pressure is measured as P1 and N2Enters the system through a pressure charging valve V5. The material evaporates and sends out light component in evaporating system, and evaporating system includes temperature monitoring system T1, and charge level indicator L2, and the thick liquid sediment after evaporating system concentration is carried to thick liquid sediment transmitting system through unloading valve V2, and transmitting system is connected with charge level indicator L1, densimeter D1 (or the integrative gamma ray charge level indicator of charge level L1 and density D1), and the solid content value A1 who calculates. And the slurry slag after the evaporation treatment enters a sending system, and then a slurry slag discharging procedure is carried out according to the solid content value of the slurry slag, so that the slurry slag is uniformly and stably discharged to a slurry slag treatment system through a discharge valve V3.
Example 1
(1) The method comprises the following steps of (1) initializing, manually discharging slurry slag for 2 times after a monomer synthesis device is started to normally produce, and automatically recording the discharge time interval and the solid content of the slurry slag discharged by a sending tank by an automatic program;
(2) a waiting step, namely, after the slurry slag is conveyed, putting a solid content automatic slurry slag discharging program, inputting a slurry slag solid content discharging target value of 50%, wherein the initial discharging interval is 5 hours, automatically calculating the slurry slag discharging time interval according to the slurry slag solid content program, and starting a slurry slag filling step when the timing time interval is reached;
(3) filling: detecting that V2, V3, V4 and V5 are in a closed state; opening V4, waiting for 60s, and starting timing the next slurry slag discharge time interval; opening the V2, conveying the materials in the evaporation system to the sending system, closing the V2 when the material level of the sending tank reaches 80% of the set material level value, waiting for 60s, displaying and recording the solid content of the sending tank at this time, and calculating the next slurry and slag discharge time interval;
(4) a sending step: closing the V4, and opening the V5 for pressurizing; when P1 reaches a set pressure sending value of 3bar, V3 is opened for sending, and when the material level of a sending tank reaches a set value of 5%, V5 is closed after timing for 60 s; when the pressure of P1 is reduced to 0.5bar, V3 is closed, V3 is closed, and the transmission is finished;
(5) and (5) continuing to wait for the next discharge time interval to reach, and repeating the steps (2) to (4).
Table 1 is a statistical table of the automatically discharged slurry slag of example 1 in which the set value of the target solid content is 50%
TABLE 1
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | 8.9 |
2 | Average discharged solid content | % | 50.5 |
3 | Discharge capacity | kg/t monomer | 14.8 |
4 | Number of blockages | Sub/production cycle | 0 |
The discharge amount is the mass of silane slurry slag discharged per ton of chlorosilane monomer produced.
Example 2
The other steps are identical to example 1, except that the solids target set point is 45%. Table 2 is a statistical table of the automatically discharged slurry slag of example 2 with a target set value of solid content of 45%:
TABLE 2
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | 12.1 |
2 | Average discharged solid content | % | 45.2 |
3 | Discharge capacity | kg/t monomer | 17.6 |
4 | Number of blockages | Sub/production cycle | 0 |
Example 3
The other steps are identical to those of example 1, except that the target solid content set value is 55%, and the set sending pressure value in the automatic program sending step is optimized to 4.2 bar. Table 3 is a statistical table of the automatically discharged slurry slag with the target set value of the solid content of 55% in example 3:
TABLE 3
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | 6.7 |
2 | Average discharged solid content | % | 55.1 |
3 | Discharge capacity | kg/t monomer | 11.8 |
4 | Number of blockages | Sub/production cycle | 0 |
Example 4
The other steps are identical to those of example 1, except that the target solid content set value is 60%, and the set sending pressure value in the automatic program sending step is optimized to 5 bar. Table 4 is a statistical table of the automatically discharged slurry slag of example 4 with a target set value of solid content of 60%:
TABLE 4
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | 6 |
2 | Average discharged solid content | % | 60.2 |
3 | Discharge capacity | kg/t monomer | 10.1 |
4 | Number of blockages | Sub/production cycle | 3 |
The test was stopped after 1 shift due to frequent clogging problems.
Comparative example 1
According to the prior art of the invention, slurry and slag are manually discharged according to the material level and the temperature of an evaporation system, and the specific operation specification is as follows: when the material level of the evaporation system reaches 80 percent and the evaporation temperature reaches 160 ℃, manually feeding the slurry slag tank, and closing the feeding when the material level of the evaporation system is reduced to 75 percent. The statistics are shown in Table 5.
TABLE 5
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | / |
2 | Average discharged solid content | % | / |
3 | Discharge capacity | kg/t monomer | 24.4 |
4 | Number of blockages | Sub/production cycle | 3 |
Comparative example 2
According to the prior art, the discharge time interval is manually set to discharge the slurry slag, the discharge interval is set according to the early stage, the middle stage and the later stage of the reaction time, the average value is 0.9 hour and 1 time, and the statistics of the discharged slurry slag are shown in a table 6.
TABLE 6
Serial number | Item | Unit of | |
1 | Number of discharges | Sub/class | 13.3 |
2 | Average discharged solid content | % | 38.5 |
3 | Discharge capacity | kg/t monomer | 19.8 |
4 | Number of blockages | Sub/production cycle | 2 |
After the method for automatically discharging the silane slurry slag according to the solid content is put into use, the discharge amount of the silane slurry slag is effectively reduced, the blocking times in the production process are further reduced, the utilization rate of raw materials is improved, the cost for treating the discharged slurry slag can be reduced, energy is saved, and the environment is protected.
The above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the embodiments of the present invention, and those skilled in the art can easily make various changes or modifications according to the main concept and spirit of the present invention, so the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (12)
1. A method for automatically discharging silane slurry slag according to solid content comprises the following steps: the materials separated from the heavy components by the washing tower enter an evaporation system, the evaporation system is heated to evaporate the light components, the slurry and slag concentrated by the evaporation system are conveyed to a slurry and slag sending system, and then the slurry and slag are discharged; wherein the discharge time interval of the slurry slag in the sending system is calculated according to a formula shown in a formula (I):
Tn=Tn-1+Tn-1×(P0-Pn-1)/P0 (I)
wherein n is the number of times of discharging the slurry slag, n is more than or equal to 1, TnIs the slurry and slag discharge time interval, T, of the nth operationn-1Is the slurry and slag discharge time interval P of the n-1 th operation0Is the target set value of the solid content of the slurry slag, Pn-1Is the solid content of the slurry residue in the n-1 st operation, and when n is 1, T isn-1Is T0,T0The initial discharge time interval of the slurry slag is set.
2. The method according to claim 1, characterized in that the set point P of the solids content of the sludge is a target value030-60%; and/or at the time of initial discharge of set sludgeInterval T0When the ratio is 3-8.
3. The method according to claim 2, characterized in that the set point P of the solids content of the sludge is a target value045-55%, setting the initial discharge time interval T of the slurry slag0For 4-6 hours.
4. The method of claim 1, wherein the vaporization system comprises a vaporization tank, a temperature monitoring system, a level gauge; the silane slurry slag is continuously discharged from the washing tower and enters the evaporation system through the feeding valve, the evaporation system intermittently discharges materials to the sending system, the evaporation system is connected with the sending system through the discharging pipe and the pressure equalizing pipe, the pressure equalizing pipe is provided with a pressure equalizing valve, the pressure equalizing pipe is connected with a pressure charging pipeline provided with the pressure charging valve, the pressure equalizing valve is used for balancing the pressure of the evaporation system and the pressure of the sending system, and the pressure charging valve is used for charging inert gas.
5. The method as claimed in claim 1, wherein the evaporation system is operated at a temperature of 120 ℃. about.200 ℃.
6. The method as claimed in claim 5, wherein the evaporation system is operated at a temperature of 150 ℃ and 180 ℃.
7. The method of claim 1, wherein the sending system comprises a sending tank, a level gauge, a density gauge.
8. The method of claim 7, wherein the level gauge and the density gauge are gamma ray level gauges integrated with the level gauge and the density gauge.
9. The method of claim 1, wherein the discharge interval of the discharged slurry slag in the sending system is calculated based on a solid content of the slurry slag, wherein the solid content is calculated as shown in the following equation (II):
wherein the D1 discharge system measures the pulp residue density, the solid density in D2 pulp residue and the liquid density in D3 pulp residue; wherein the solid density is calculated by referring to the composition of the fine powder collected by the cyclone; the liquid density is calculated by the liquid phase composition of the slurry residue; the density of the slurry slag is measured by gamma ray.
10. The method of claim 1, wherein the delivery system is operated at a pressure of 2 to 5bar when pressurized; at the end of the discharge, the system pressure is 0.2-1.0 bar.
11. The method of claim 10, wherein the system pressure is 3-4bar when charging; at the end of the discharge, the system pressure is 0.3-0.7 bar.
12. The method for automatically discharging silane paste slag according to solid content as claimed in claim 1, comprising the steps of:
(1) the method comprises the following steps that in the initial step, after the monomer synthesis device is started to normally produce, a system for automatically discharging the slurry slag according to the solid content is started to be used, and the automatic program automatically records the discharge time interval and the solid content of the slurry slag discharged by a sending tank;
(2) a waiting step, after the slurry slag is conveyed to a sending system, calculating the time interval of the slurry slag discharging according to a formula (I), and starting the slurry slag filling step when the timing time interval is reached;
(3) filling: opening a pressure equalizing valve of the evaporation system, waiting for 30-60s, starting timing of the next slurry and slag discharge time interval, opening a blanking valve between the evaporation system and the sending system, conveying the material in the evaporation system to the sending system, closing the blanking valve when the material level of the sending tank reaches 70-100% of the material level, waiting for 30-60s, recording the slurry and slag density in the sending tank, and further calculating the solid content of the slurry and slag;
(4) a sending step: closing the pressure equalizing valve, opening the pressurizing valve, pressurizing to 2-5bar, opening the discharging valve for discharging, waiting for 30-60s when the material level of the sending tank reaches 5-10% of the material level, closing the pressurizing valve, closing the discharging valve when the system pressure is reduced to 0.3-0.7bar, ending the sending program, continuing waiting for the next time of discharging time interval, timing, and repeating the step (2) -the step (4).
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US3249147A (en) * | 1962-07-03 | 1966-05-03 | Burnett & Rolfe Ltd | Film evaporators |
CN205516609U (en) * | 2016-03-30 | 2016-08-31 | 东阿阿胶股份有限公司 | Production of cream side is with small -size concentration machine set that draws |
CN109897058A (en) * | 2019-02-28 | 2019-06-18 | 天津大学 | An organosilicon slurry slag treatment system and treatment process |
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US3249147A (en) * | 1962-07-03 | 1966-05-03 | Burnett & Rolfe Ltd | Film evaporators |
CN205516609U (en) * | 2016-03-30 | 2016-08-31 | 东阿阿胶股份有限公司 | Production of cream side is with small -size concentration machine set that draws |
CN109897058A (en) * | 2019-02-28 | 2019-06-18 | 天津大学 | An organosilicon slurry slag treatment system and treatment process |
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