CN111632469A - Dust-containing waste gas interception process and device in organic silicon monomer production - Google Patents
Dust-containing waste gas interception process and device in organic silicon monomer production Download PDFInfo
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- CN111632469A CN111632469A CN202010386652.9A CN202010386652A CN111632469A CN 111632469 A CN111632469 A CN 111632469A CN 202010386652 A CN202010386652 A CN 202010386652A CN 111632469 A CN111632469 A CN 111632469A
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- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
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Abstract
The invention belongs to the technical field of waste gas treatment, and particularly relates to a process and a device for intercepting dust-containing waste gas in organosilicon monomer production, which comprises a solvent washing tower, a solvent reflux tank, a reflux condenser, a waste gas intercepting condenser, a demister and a water washing tower, wherein the waste gas is washed and intercepted by using a byproduct generated by a monomer synthesis process as a solvent, the physicochemical property of the adopted byproduct washing solvent is similar to the physicochemical property of harmful gas in the waste gas, the washing and recovery of the harmful gas are easier to realize according to the similar intermiscibility principle, most of the harmful gas and fine powder in the waste gas after solvent washing are intercepted, the yield of hydrolysate at the bottom of the water washing tower and the consumption of a neutralizer are greatly reduced, the labor intensity of cleaning the water washing tower is reduced, the production cost is reduced, meanwhile, the full recycling of liquid phase components can be realized, and the waste of raw materials is reduced, the solid phase can be used for extracting copper, and high-value recycling of materials is realized.
Description
Technical Field
The invention belongs to the technical field of waste gas treatment, and particularly relates to a process and a device for intercepting dust-containing waste gas in organic silicon monomer production.
Background
At present, methyl chloride and silicon powder are generally adopted at home and abroad to directly synthesize methyl chlorosilane monomers under the catalysis of a copper system, the main product of the methyl chlorosilane monomers produced by a direct method is dimethyl dichlorosilane, the selectivity of the dimethyl dichlorosilane in the reaction is generally between 80% and 90% (the selectivity is mainly based on the condition of the process, the process technology at home and abroad is generally mature compared with that at home, for the domestic process, the selectivity of the dimethyl dichlorosilane is generally only stabilized to 80% to 85%, the content of byproducts is mainly methyl trichlorosilane, the content of trimethyl chlorosilane and methyl hydrogen dichlorosilane is about 5% to 15%, the content of high boiling point mixture is about 1% to 8%, and the content of low boiling point mixture (the boiling point is lower than 40 ℃) is about 1% to 2%.
The by-product in the production of the organic silicon monomer is easy to react with moisture in the air to generate hydrogen chloride, and can cause huge pollution to the ecological environment in the discharging and storing processes. With further scale-up of the production of organosilicon monomers, the absolute amount of by-products is considerable.
A large amount of dust-containing waste gas is generated in the production process of the organic silicon monomer, the harmful gas in the waste gas is mainly chlorosilane gas, and the dust is silicon-copper mixed fine powder. The waste gas treatment mode of the organosilicon monomer synthesis process generally adopts a mode of combining water washing waste gas and alkali washing waste gas, and essentially causes water and chlorosilane gas to generate chemical reaction. As a result, a large amount of hydrolysate and acid water are produced at the bottom of the water washing tower, and a large amount of fine powder is coated. These hydrolysates are viscous and very difficult to handle, and the water washing process also consumes a large amount of water resources and generates a large amount of waste acid. In order to realize the recycling of water, a large amount of neutralizing agents are needed to realize the acidity regulation, and the waste gas treatment mode is more and more difficult to adapt to the current environmental protection requirement.
Patent CN207287070U discloses an organosilicon monomer rectification vent tail gas treatment device, which comprises three layers of packing layers and adopts water as a washing agent, no matter how high the tail gas treatment effect of such a device is, sticky hydrolysate in the tail gas is adhered to the packing, thereby causing the device to be blocked. The frequency and cost of filler replacement for such devices can be high, and the filler is difficult to reuse, and the cost of the tail gas absorption device is too high.
The same tail gas treatment principle, namely water is used as a washing agent, a tower or a pool container is adopted in the patents CN103007717A, CN207042196U, CN206867987U, CN206262339U and CN208599406U, a monomer in the tail gas is reacted with water to generate a hydrolysate, and acid water is neutralized with alkali to realize the absorption treatment of the tail gas. These patents have the disadvantage that the tail gas absorption devices used are relatively complex; as with patent CN207287070U, it also faces the difficulty of adhering the hydrolyzat to the equipment, which is difficult to clean; the water washing process, i.e., hydrolysis process, consumes a large amount of water, and a large amount of neutralizing base is required for neutralizing the acid water produced.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects of the prior art are overcome, the dusty waste gas interception process and the device in the production of the organic silicon monomer are provided, the harmless treatment of the waste gas is realized by adopting the similarity intermiscibility principle, the generation of hydrolysate and waste acid is reduced, the occurrence of secondary pollutants is avoided, the labor intensity is reduced, the raw materials are recovered, and the production cost is reduced.
The device for intercepting the dust-containing waste gas in the production of the organic silicon monomer comprises a dust-containing waste gas pipeline, wherein the dust-containing waste gas pipeline is connected with the bottom of a solvent washing tower, the bottom of the solvent washing tower is connected with a solvent reflux tank, the bottom of the solvent reflux tank is connected with a reflux condenser through a circulating pump, the reflux condenser is connected with the top of the solvent washing tower, the top of the solvent washing tower is connected with an intercepting waste gas condenser, and the intercepting waste gas condenser is sequentially connected with a demister and a water washing tower.
Preferably, the bottom of the solvent reflux tank is connected with a post-treatment device of the monomer synthesis system, so that all liquid-phase components can be recycled, the waste of raw materials is reduced, and the solid phase can be used for extracting copper, so that high-value recycling of materials is realized.
The invention relates to a process for intercepting dust-containing waste gas in the production of organosilicon monomers, which comprises the following steps:
(1) introducing the dust-containing waste gas into a solvent washing tower from the bottom of the solvent washing tower through a dust-containing waste gas pipeline, pumping the solvent in a solvent reflux tank to a reflux condenser through a circulating pump, condensing the solvent, and then introducing the condensed solvent into the top of the solvent washing tower to wash and intercept the waste gas;
(2) after washing and intercepting, the mixture at the bottom of the solvent washing tower automatically overflows into a solvent reflux tank, part of the mixture in the solvent reflux tank is used for circulation, part of the mixture enters a post-treatment device of a monomer synthesis system to recycle all liquid phase components, high-valued recycling of the materials is realized, the solvent is replenished after part of the washed mixture is discharged, and the liquid level of the solvent reflux tank is kept unchanged;
(3) and the intercepted waste gas enters the water washing tower from the top of the solvent washing tower through the waste gas intercepting condenser and the demister, the waste gas is subjected to final purification treatment, and then the waste gas reaches the standard and is discharged.
The solvent is a byproduct generated in the production process of the organic silicon monomer, and preferably all liquid phase byproducts.
In the step (1), the solvent washing tower and the solvent reflux tank are filled with 20-80% of solvent, preferably 30-70% of solvent before use. The liquid levels of the solvent washing tower and the solvent reflux tank cannot be too high, the phenomenon that the liquid level rises quickly can occur after waste gas is introduced into the tower bottom, the too high liquid level can overflow the washing tower, a large amount of liquid is contained in a tower outlet and a pipeline behind the tower outlet, and the washing effect is obviously reduced.
The refrigerant of the reflux condenser adopts circulating water, and the temperature is 5-50 ℃, preferably 15-35 ℃.
The refrigerant of the waste gas intercepting condenser is ethylene glycol, and the temperature is-20-5 ℃, preferably-15-0 ℃.
And (3) in the step (2), when the mass content of the light components in the solvent reflux tank is 5-35% and the content reaches 35 wt% or more, discharging part of materials to a post-treatment device of the monomer synthesis system to prevent the washing effect from being weakened. The discharged materials can realize the full recycling of liquid phase components, the waste of raw materials is reduced, and the solid phase can be used for extracting copper, thereby realizing the high-valued recycling of the materials.
The main components of the dust-containing waste gas in the step (1) are as follows: nitrogen, a gas phase chlorosilane mixture, fine powders of silicon and copper, and the like. Wherein the gas phase chlorosilane mixture, silicon and copper fine powder can be intercepted.
The interception process of the dust-containing waste gas in the production of the organic silicon monomer can be used for treating all waste gas and dust-containing waste gas generated in the synthesis process (the driving process and the stopping process) of the organic silicon monomer.
Compared with the prior art, the invention has the following beneficial effects:
1. the solvent adopted by the invention is derived from byproducts generated by a monomer synthesis process, other solvents are not introduced, the method belongs to the reutilization of the byproducts, the cost of the washing solvent is almost zero, and the method conforms to the concept of green environmental protection.
2. The physicochemical property of the byproduct washing solvent adopted by the invention is similar to that of harmful gas (gas-phase chlorosilane mixture) in the waste gas, and the washing and recovery of the harmful gas can be more easily realized according to the similar intermiscibility principle.
3. Most harmful gases and fine powder in the waste gas after solvent washing are intercepted, so that the yield of hydrolysate and the using amount of a neutralizer at the bottom of the water washing tower are greatly reduced, the labor intensity for cleaning the water washing tower is reduced, and the production cost is reduced.
4. Harmful gas and fine powder intercepted in the waste gas are absorbed in the washing solvent, the washing solvent returns to a post-treatment device of the monomer synthesis system, so that the full recycling of liquid phase components can be realized, the waste of raw materials is reduced, and the solid phase can be used for extracting copper, so that the high-valued recycling of materials is realized.
5. The production device provided by the invention has the advantages of simple structure, scientificity, reasonability, high production efficiency, energy conservation and environmental protection.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1. a dusty waste gas line; 2. a solvent wash column; 3. a solvent reflux tank; 4. a post-processing device; 5. a circulation pump; 6. a reflux condenser; 7. intercepting a waste gas condenser; 8. a demister; 9. and (5) washing the tower with water.
Detailed Description
The invention is further described with reference to the following figures and examples.
The hydrolysate is produced by reacting the gas phase chlorosilane mixture with water in the waste gas, and contains a large amount of fine powder. Therefore, the interception recovery capability of the waste gas can be measured by the amount of the hydrolysate. The interception rate is (amount of the hydrolysate in the water washing pool without interception-amount of the hydrolysate in the water washing pool after interception)/amount of the hydrolysate in the water washing pool without interception. The measurement samples of the interception rate used the same production cycle: for example, the sample test with the interception period of 10 days and the sample test with the non-interception period of 10 days.
Example 1
As shown in fig. 1, dusty waste gas pipeline 1 be connected with solvent scrubber 2 bottom, the bottom and the solvent reflux groove 3 of solvent scrubber 2 are connected, solvent reflux groove 3 bottom is connected with reflux condenser 6 through circulating pump 5, solvent reflux groove 3 bottom still be connected with aftertreatment device 4, reflux condenser 6 with solvent scrubber 2 top is connected, solvent scrubber 2 top is connected with interception waste gas condenser 7, interception waste gas condenser 7 is connected with defroster 8 and rinsing tower 9 in proper order.
Byproducts generated in the synthesis process of the organic silicon monomer are injected into a tower kettle of a solvent washing tower 2 and a solvent reflux tank 3, and the liquid levels are 30% and 55% respectively. Introducing dust-containing waste gas from the bottom of the solvent washing tower 2 through a dust-containing waste gas pipeline 1, and starting a circulating pump 5 to continuously reflux. The washed gas enters a water washing tower 9 through a waste gas intercepting condenser 7 and a demister 8. After the solvent is washed for a period of time, when the light component content in the solvent mixture is measured to reach 35% by taking the liquid phase in the solvent reflux tank 3, discharging a part of the solvent mixture in the solvent reflux tank 3 to a post-treatment device 4 of the monomer synthesis system, and then supplementing a part of by-products to keep the liquid level of the solvent reflux tank 3 at 55%. And (3) carrying out sequential circulation operation for 10 days, collecting 3 tons of hydrolysate in total, supplementing 6 tons of water into the washing tank, supplementing 3 tons of neutralizing agent, and keeping the acidity of water in the washing tank neutral. The period of not putting into the solvent washing tower 2 is 10 days, 18.9 tons of hydrolysate is collected in total, 20 tons of water is added into the water washing pool, and 7 tons of neutralizing agent is added to keep the acidity of the water washing pool neutral. The interception rate of harmful gas and powder in the waste gas is about: (18.9-3)/18.9-84.13%.
Example 2
As shown in fig. 1, dusty waste gas pipeline 1 be connected with solvent scrubber 2 bottom, the bottom and the solvent reflux groove 3 of solvent scrubber 2 are connected, solvent reflux groove 3 bottom is connected with reflux condenser 6 through circulating pump 5, solvent reflux groove 3 bottom still be connected with aftertreatment device 4, reflux condenser 6 with solvent scrubber 2 top is connected, solvent scrubber 2 top is connected with interception waste gas condenser 7, interception waste gas condenser 7 is connected with defroster 8 and rinsing tower 9 in proper order.
Byproducts generated in the synthesis process of the organic silicon monomer are injected into a tower kettle of a solvent washing tower 2 and a solvent reflux tank 3, and the liquid levels are 35% and 60% respectively. Introducing dust-containing waste gas from the bottom of the solvent washing tower 2 through a dust-containing waste gas pipeline 1, and starting a circulating pump 5 to continuously reflux. The washed gas enters a water washing tower 9 through a waste gas intercepting condenser 7 and a demister 8. After the solvent is washed for a period of time, when the light component content in the solvent mixture is measured to reach 35% by taking the liquid phase of the solvent reflux tank 3, discharging a part of the solvent mixture in the solvent reflux tank 3 to a post-treatment device 4 of the monomer synthesis system, and then supplementing a part of by-products to keep the liquid level of the solvent reflux tank 3 at 60%. And (3) performing sequential circulation operation for 10 days, collecting 2.6 tons of hydrolysate in total, supplementing 4 tons of water and 2 tons of neutralizing agent into the washing tank, and keeping the acidity of water in the washing tank neutral. The period of not putting into the solvent washing tower 2 is 10 days, 17.2 tons of hydrolysate is collected in total, 18 tons of water is added into the water washing pool, and 8 tons of neutralizing agent is added to keep the acidity of the water washing pool neutral. The interception rate of harmful gas and powder in the waste gas is about: (17.2-2.6)/17.2-84.88%.
Example 3
As shown in fig. 1, dusty waste gas pipeline 1 be connected with solvent scrubber 2 bottom, the bottom and the solvent reflux groove 3 of solvent scrubber 2 are connected, solvent reflux groove 3 bottom is connected with reflux condenser 6 through circulating pump 5, solvent reflux groove 3 bottom still be connected with aftertreatment device 4, reflux condenser 6 with solvent scrubber 2 top is connected, solvent scrubber 2 top is connected with interception waste gas condenser 7, interception waste gas condenser 7 is connected with defroster 8 and rinsing tower 9 in proper order.
Byproducts generated in the synthesis process of the organic silicon monomer are injected into a tower kettle of a solvent washing tower 2 and a solvent reflux tank 3, and the liquid levels are 40% and 65% respectively. Introducing dust-containing waste gas from the bottom of the solvent washing tower 2 through a dust-containing waste gas pipeline 1, and starting a circulating pump 5 to continuously reflux. The washed gas enters a water washing tower 9 through a waste gas intercepting condenser 7 and a demister 8. After the solvent is washed for a period of time, when the light component content in the solvent mixture is measured to reach 35% by taking the liquid phase in the solvent reflux tank 3, discharging a part of the solvent mixture in the solvent reflux tank 3 to a post-treatment device 4 of the monomer synthesis system, and then supplementing a part of by-products to keep the liquid level of the solvent reflux tank 3 at 65%. And (4) sequentially and circularly operating for 10 days, collecting 0.8 ton of hydrolysate in total, supplementing 4 tons of water and 1.5 tons of neutralizing agent into the washing tank, and keeping the acidity of water in the washing tank neutral. The period of not putting into the solvent washing tower 2 is 10 days, 15.68 tons of hydrolysate is collected in total, 15 tons of water is added into the water washing pool, and 5 tons of neutralizing agent is added to keep the acidity of the water washing pool neutral. The interception rate of harmful gas and powder in the waste gas is about: (15.68-0.8)/15.68 ═ 94.90%.
Example 4
As shown in fig. 1, dusty waste gas pipeline 1 be connected with solvent scrubber 2 bottom, the bottom and the solvent reflux groove 3 of solvent scrubber 2 are connected, solvent reflux groove 3 bottom is connected with reflux condenser 6 through circulating pump 5, solvent reflux groove 3 bottom still be connected with aftertreatment device 4, reflux condenser 6 with solvent scrubber 2 top is connected, solvent scrubber 2 top is connected with interception waste gas condenser 7, interception waste gas condenser 7 is connected with defroster 8 and rinsing tower 9 in proper order.
By-products generated in the synthesis process of the organic silicon monomer are injected into a tower kettle of a solvent washing tower 2 and a solvent reflux tank 3, and the liquid levels are 45% and 70% respectively. Introducing dust-containing waste gas from the bottom of the solvent washing tower 2 through a dust-containing waste gas pipeline 1, and starting a circulating pump 5 to continuously reflux. The washed gas enters a water washing tower 9 through a waste gas intercepting condenser 7 and a demister 8. After the solvent is washed for a period of time, when the light component content in the solvent mixture is measured to reach 35% by taking the liquid phase of the solvent reflux tank 3, discharging a part of the solvent mixture in the solvent reflux tank 3 to a post-treatment device 4 of the monomer synthesis system, and then supplementing a part of by-products to keep the liquid level of the solvent reflux tank 3 at 70%. And (3) performing sequential circulation operation for 10 days, collecting 1 ton of hydrolysate in total, supplementing 3 tons of water into the water washing pool, supplementing 1 ton of neutralizing agent, and keeping the acidity of water in the water washing pool neutral. The period of not putting into the solvent washing tower 2 is 10 days, 17.1 tons of hydrolysate is collected in total, 15 tons of water are added into the water washing pool, and 6 tons of neutralizing agent are added to keep the acidity of the water washing pool neutral. The interception rate of harmful gas and powder in the waste gas is about: (17.1-1)/17.1 ═ 94.15%.
Example 5
As shown in fig. 1, dusty waste gas pipeline 1 be connected with solvent scrubber 2 bottom, the bottom and the solvent reflux groove 3 of solvent scrubber 2 are connected, solvent reflux groove 3 bottom is connected with reflux condenser 6 through circulating pump 5, solvent reflux groove 3 bottom still be connected with aftertreatment device 4, reflux condenser 6 with solvent scrubber 2 top is connected, solvent scrubber 2 top is connected with interception waste gas condenser 7, interception waste gas condenser 7 is connected with defroster 8 and rinsing tower 9 in proper order.
Byproducts generated in the synthesis process of the organic silicon monomer are injected into a tower kettle of a solvent washing tower 2 and a solvent reflux tank 3, and the liquid levels are 40% and 65% respectively. Introducing dust-containing waste gas from the bottom of the solvent washing tower 2 through a dust-containing waste gas pipeline 1, and starting a circulating pump 5 to continuously reflux. The washed gas enters a water washing tower 9 through a waste gas intercepting condenser 7 and a demister 8. After the solvent is washed for a period of time, when the light component content in the solvent mixture is measured to reach 35% by taking the liquid phase in the solvent reflux tank 3, discharging a part of the solvent mixture in the solvent reflux tank 3 to a post-treatment device 4 of the monomer synthesis system, and then supplementing a part of by-products to keep the liquid level of the solvent reflux tank 3 at 65%. And (3) performing sequential circulation operation for 10 days, collecting 1.1 tons of hydrolysate in total, supplementing 4 tons of water into the water washing pool, supplementing 1 ton of neutralizing agent, and keeping the acidity of water in the water washing pool neutral. The period of not putting into the solvent washing tower 2 is 10 days, 18.1 tons of hydrolysate is collected in total, 14 tons of water are added into the water washing pool, and 7.8 tons of neutralizing agent are added to keep the acidity of the water washing pool neutral. The interception rate of harmful gas and powder in the waste gas is about: (18.1-1.1)/18.1-93.92%.
The process parameters and the interception rates of examples 1-5 are shown in Table 1.
Table 1 examples 1-5 process parameters and intercept rates
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (8)
1. A dust-containing waste gas interception process in organosilicon monomer production is characterized in that: the method comprises the following steps:
(1) introducing dust-containing waste gas into the solvent washing tower (2) from the bottom of the solvent washing tower (2) through a dust-containing waste gas pipeline (1), pumping the solvent in the solvent reflux tank (3) to a reflux condenser (6) through a circulating pump (5), condensing the solvent, and then introducing the condensed solvent to the top of the solvent washing tower (2) to wash and intercept the waste gas;
(2) after washing and intercepting, the mixture at the bottom of the solvent washing tower (2) automatically overflows into a solvent reflux tank (3), part of the mixture in the solvent reflux tank (3) is used for circulation, part of the mixture enters a post-treatment device (4) of a monomer synthesis system to recycle all liquid phase components, and after part of the washed mixture is discharged, the solvent is replenished, and the liquid level of the solvent reflux tank (3) is kept unchanged;
(3) the intercepted waste gas enters a water washing tower (9) from the top of the solvent washing tower (2) through an intercepted waste gas condenser (7) and a demister (8), the waste gas is subjected to final purification treatment, and then the waste gas is discharged after reaching the standard.
2. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: the solvent is a byproduct generated in the production process of the organic silicon monomer.
3. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: in the step (1), 20-80% of solvent is added into the solvent washing tower (2) and the solvent reflux tank (3) before the solvent washing tower and the solvent reflux tank are put into service.
4. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: the refrigerant of the reflux condenser (6) adopts circulating water, and the temperature is 5-50 ℃.
5. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: the refrigerant of the waste gas intercepting condenser (7) is ethylene glycol, and the temperature is-20-5 ℃.
6. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: and (3) when the content of light components in the solvent reflux tank (3) in the step (2) reaches 35 wt% or more, discharging part of materials to a post-treatment device (4) of the monomer synthesis system.
7. The process for intercepting dust-containing waste gases in the production of organosilicon monomers according to claim 1, wherein: used for treating all waste gas and dust-containing waste gas generated in the synthesis process of the organic silicon monomer.
8. A process unit for intercepting dust-containing waste gas in the production of organosilicon monomers as claimed in claim 1, comprising a dust-containing waste gas line (1), characterized in that: dusty waste gas pipeline (1) be connected with solvent scrubbing tower (2) bottom, the bottom and the solvent reflux groove (3) of solvent scrubbing tower (2) are connected, solvent reflux groove (3) bottom is connected with reflux condenser (6) through circulating pump (5), solvent reflux groove (3) bottom be connected with aftertreatment device (4), reflux condenser (6) with solvent scrubbing tower (2) top is connected, solvent scrubbing tower (2) top is connected with interception waste gas condenser (7), interception waste gas condenser (7) are connected with defroster (8) and scrubbing tower (9) in proper order.
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| CN114247265A (en) * | 2021-11-29 | 2022-03-29 | 鲁西化工集团股份有限公司硅化工分公司 | System and method for purifying and recycling organic silicon emptying tail gas |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114247265A (en) * | 2021-11-29 | 2022-03-29 | 鲁西化工集团股份有限公司硅化工分公司 | System and method for purifying and recycling organic silicon emptying tail gas |
| CN114247265B (en) * | 2021-11-29 | 2024-05-24 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon emptying tail gas purifying and recycling treatment system and method |
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