CN101456877A - Contact masses processing method during methylchlorosilane synthesis - Google Patents
Contact masses processing method during methylchlorosilane synthesis Download PDFInfo
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- CN101456877A CN101456877A CNA2008102430916A CN200810243091A CN101456877A CN 101456877 A CN101456877 A CN 101456877A CN A2008102430916 A CNA2008102430916 A CN A2008102430916A CN 200810243091 A CN200810243091 A CN 200810243091A CN 101456877 A CN101456877 A CN 101456877A
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Abstract
The invention relates to the field of organic chemistry, in particular to a method for processing and recovering contacts in the synthetic process of methyl chlorosilane, which is characterized by comprising the following steps: adding an intermediate storage tank of the contacts in the process of synthesizing the methyl chlorosilane; when the selectivity of a target product is reduced to between 70 and 90 percent, transferring the contacts in the reaction system to the intermediate storage tank; re-adding new contacts to react in a fluidized bed, and mixing the transferred contacts with fresh silicon powder; and returning the mixture to the fluidized bed to use the mixture as new contacts to be added to the reaction. In the invention, the production method is used to not only ensure the stability of the selectivity for dimethyl dichlorosilane in the synthetic process of the methyl chlorosilane, and prolong the synthetic cycle of organochlorosilane simultaneously. The effective production time of the production device can be up to over 50 days.
Description
Technical field
The present invention relates to organic chemistry filed, be specifically related to the processing recovery method of contact in a kind of methyl chlorosilane building-up process.
Background technology
Methyl chlorosilane is the most important intermediate raw material of preparation organosilicon polymer, also is the basic raw material of producing other functionalized silicon base silanes.Wherein, account for 90% of methyl chlorosilane with the consumption maximum of dimethyldichlorosilane(DMCS) (M2).Therefore, domestic and international organosilyl manufacturing enterprise all with the optionally height of dimethyldichlorosilane(DMCS) as the performance assessment criteria of combined coefficient quality, simultaneously the length of synthesis cycle also is reduced to a certain degree with the selectivity of dimethyldichlorosilane(DMCS) and weighs, guaranteeing that M2 has under the higher optionally prerequisite, the level of long more explanation synthesis technique of synthetic production cycle is higher, the synthesizer reason that also heals.
In fluidized-bed reactor, silica flour and copper powder mix the active contact of formation, prolongation along with the reaction times, the settling on contact surface can get more and more, mainly increase because of accumulating carbon-containing impurities and then pollution silicon bronze body contacts and some other waste material in the reaction process, make the active reduction of contact, side reaction strengthens, and causes the M2 selectivity to reduce.At present, both at home and abroad the organochlorosilane production equipment when the selectivity of dimethyldichlorosilane(DMCS) is reduced to economic stagnation point, i.e. parking maintenance.At this moment, waste catalyst need be discharged reactor, and reaction vessel must be cleared up cleaning.Just can add new contact after reactor cleans and clears up again and carry out the continous-stable reaction, begin the production of new one-period.The production cycle of organosilicon manufacturer was generally 25～30 days.After this generally need about 3 days time of cost to overhaul.Overhaul of the equipments has influenced the effective production time of methyl chlorosilane device greatly, and then influences economic benefit of enterprises.In addition, because the waste catalyst median size is thinner, contain highly active copper, on the one hand, it is exposed in the air can cause oxidation even burning, if untimely dealing carefully with can be caused serious pollution to environment, has potential safety hazard; On the other hand, cause the significant wastage of silicon and copper.
Summary of the invention
The invention discloses the method that the contact processing is recycled in a kind of methyl chlorosilane synthetic reaction process.The present invention is guaranteeing that M2 has the higher effective production time that optionally makes device simultaneously and extends to more than 50 days, and the turnaround of unit time still only needs 3-4 days time, this has just made full use of the methyl chlorosilane production equipment, increase effective production time, increase the annual production of methyl silicon chlorosilane, help improving the business economic benefit.
The method of synthesizing methyl-chloro-silane of the present invention, comprise and partly to add fluidized-bed by the active contact that silica flour and copper powder are formed, feed unstripped gas, react after gas fluidized, reacting coarse product is directly discharged from syngas outlet, the reacting coarse product fractionation gets target product, in the reaction along with the decline of bed height, uninterrupted active contact and the promotor of replenishing, feature of the present invention is: add relay tank between cyclonic separator and fluidized-bed, when the selectivity of target product is reduced to 70-85%, contact in the reactive system is transferred to relay tank, again replenish active contact in the fluidized-bed and react, can be treated or directly bed add in the reaction with returning again after active contact mixes with shifting the contact that comes out as new contact.
The preferred dimethyldichlorosilane(DMCS) of methyl chlorosilane wherein.
The preferred methyl chloride of unstripped gas wherein.
The preferred dimethyldichlorosilane(DMCS) of target product wherein.
By adding relay tank, make the contact transfer of the activity reduction of react, the contact that migrates out is treated or directly mix with active contact in production unit in the present invention, and the activity of contact is improved, and can be reused for reaction.The relay tank that adds among the present invention is preferably 2～4.
Preferably when the selectivity of dimethyldichlorosilane(DMCS) is reduced to 80-82%, the contact in the reactive system is transferred to relay tank among the present invention.The method that contact is transferred to relay tank preferably is pressed out to storage tank with nitrogen pressure with the contact in the fluidized-bed.
Contact among the present invention in the relay tank can be under logical nitrogen or air conditions heat treated, or directly to mix with active contact preferably with ratio of weight and number be 1: 0.5～5 to mix.
Adopt dual circuit to return bed system among the present invention between contact relay tank and the fluidized-bed.
Above-mentioned promotor is one or more in zinc, tin, antimony, aluminium, phosphorus, potassium, sodium preferably.
On the other hand, the contact that reacted is used for the production except improving activity again by the interpolation silica flour, can also increase a by-pass returning on the bed pipeline of contact relay tank bottom, this by-pass adopts the dual circuit system, the contact that activity reduces is sent into the synthetic fluidized-bed of trichlorosilane by pipeline, as the raw material of synthesizing trichlorosilane.All operations are undertaken by closed circuit pipeline.
Adopt production method of the present invention, both guaranteed the optionally stable of dimethyldichlorosilane(DMCS) in the methyl chlorosilane building-up process, reach the synthesis cycle that prolongs organochlorosilane simultaneously.The effective production time of production equipment can reach more than 50 days.Adopt dual circuit to return bed system among the present invention between contact relay tank and the fluidized-bed, guarantee that contact normally returns bed and do not influence ordinary production.Operations all among the present invention are all carried out in closed circuit pipeline, can avoid or reduce the pollution to environment in the production operation process, play the effect of energy-saving and emission-reduction.
Description of drawings
Fig. 1 is the synthesis technique schematic flow sheet of methyl chlorosilane
Embodiment
Embodiment 1
42 tons of active contacts of (t) (silica flour: copper powder=20:1 is weight ratio) of silica flour and copper powder add fluidized-bed in advance, by reacting after the methyl chloride fluidisation, and 280 ℃ of temperature of reaction, reaction pressure 0.3Mpa, gas speed is 0.20m/s.The gas-phase reaction product is discharged from syngas outlet, along with the decline of bed height, and continual additional active contact and promotor in reaction, promotor is the mixture of zinc powder, antimony, aluminium powder, the ratio of zinc powder, antimony, aluminium powder is 3:2:2, altogether 800kg.When being reduced to 80%, the selectivity of M2 in the synthesis gas (reacted 25 days); suspend and add contact, the contact in the fluidized-bed is pressed out in the storage tank the about 53.4t of contact with nitrogen pressure; the silica flour of collecting through cyclonic separator in the reaction process is 41.6t, the airtight protection of inflated with nitrogen.
Replenish active contact toward fluidized-bed, recover reaction conditions, 280 ℃ of temperature of reaction, reaction pressure 0.3Mpa, gas speed is 0.20m/s, repeats above-mentioned steps, and the selectivity of M2 falls after rise again to 80% (promptly reacting 24 days) in synthesis gas, it is 39.4t that cyclonic separator is collected silica flour, open the storage tank loop, in the ratio adding fluidized-bed of contact: silica flour=3:1, temperature of reaction is controlled to be 300 ℃, reaction pressure is 0.3Mpa, gas speed is 0.18m/s, adds promotor, zinc 120kg in the promotor, tin, antimony and phosphorus blending ratio are 1:1:1, altogether 20kg.Extremely the M2 selectivity is 76% o'clock (promptly reacting 4 days) in the reaction, stopped reaction, contact residue 14.2t in the storage tank, and empty in the fluidized-bed waste catalyst 48.7t to intermediate storage tank, cyclonic separator is collected fine powder 18.5t in the reaction, and storage tank 81.4t altogether enters the synthetic fluidized-bed of trichlorosilane through another piping system.This cycle produced 53 days altogether.Parking maintenance 3 days.
Embodiment 2
Silica flour and copper powder 46 tons (t) (silica flour: copper powder=22:1) is active contact, adds fluidized-bed in advance, by reacting after the methyl chloride fluidisation, and 300 ℃ of temperature of reaction, reaction pressure 0.3Mpa, gas speed is 0.18m/s.The gas-phase reaction product is discharged from syngas outlet; decline along with bed height; in reaction continual replenish fresh silica flour and copper catalyst and promotor zinc powder, antimony, aluminium powder the ratio of mixture be 2:1:1 750kg altogether; when being reduced to 79%, the selectivity of M2 in the synthesis gas (reacted 25 days); suspend and add contact; with nitrogen pressure the contact in the fluidized-bed is pressed out in the storage tank; the about 52.7t of contact; the silica flour of collecting through cyclonic separator in the reaction process is 40.8t, the airtight protection of inflated with nitrogen.
Again replenish contact toward fluidized-bed, recover reaction conditions, 300 ℃ of temperature of reaction, reaction pressure 0.3Mpa, gas speed is 0.18m/s, repeats above-mentioned steps, the selectivity of M2 falls after rise again to 79% (promptly reacting 24 days) in synthesis gas, and it is 38.4t that cyclonic separator is collected silica flour.Open the storage tank loop, contact is entered fluidized-bed through circuit system, temperature of reaction is controlled to be 330 ℃, and reaction pressure is 0.3Mpa, and gas speed is 0.15m/s, adds promotor, zinc 150kg in the promotor, and tin, antimony and phosphorus blending ratio are 1; 1:1,28kg altogether.Extremely the M2 selectivity is 75% o'clock (promptly reacting 3 days) in the reaction, stopped reaction, contact residue 41.5t in the storage tank, and empty in the fluidized-bed waste catalyst 50.2t to intermediate storage tank, cyclonic separator is collected fine powder 21.8t in the reaction, and storage tank 113.5t altogether enters the synthetic fluidized-bed of trichlorosilane through another piping system.This cycle produced 52 days altogether.Parking maintenance 3.5 days.
Claims (10)
1, a kind of method of synthesizing methyl-chloro-silane, comprise and partly to add fluidized-bed by the contact that silica flour and copper powder are formed, feed unstripped gas, react after gas fluidized, reacting coarse product is directly discharged from syngas outlet, the reacting coarse product fractionation gets target product, in the reaction along with the decline of bed height, uninterrupted silica flour and copper powder and the promotor of replenishing, it is characterized in that: between cyclonic separator and fluidized-bed, add the contact relay tank, when the selectivity of target product is reduced to 70-85%, contact in the reactive system is transferred to relay tank, replenishes new contact in the fluidized-bed again and react, bed add in the reaction as new contact with returning again after shifting the contact that comes out and fresh silica flour mixing.
2, the process of claim 1 wherein that methyl chlorosilane is a dimethyldichlorosilane(DMCS).
3, the process of claim 1 wherein that unstripped gas is methyl chloride.
4, the process of claim 1 wherein that target product is a dimethyldichlorosilane(DMCS).
5, the process of claim 1 wherein that the relay tank that adds is 2～4.
6, the process of claim 1 wherein and when the selectivity of dimethyldichlorosilane(DMCS) is reduced to 80-82%, the contact in the reactive system is transferred to relay tank.
7, the process of claim 1 wherein that shifting the contact and the fresh silica flour that come out is that mix 1:0.5～5 with the ratio of weight and number.
8, the process of claim 1 wherein that promotor is selected from one or more in zinc, tin, antimony, aluminium, phosphorus, potassium, the sodium.
9, the process of claim 1 wherein that the method that contact is transferred to relay tank is with nitrogen pressure the contact in the fluidized-bed to be pressed out to storage tank.
10, the process of claim 1 wherein between contact relay tank and fluidized-bed and to adopt the dual circuit circuit system.
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| CN102212080A (en) * | 2010-04-12 | 2011-10-12 | 中国科学院过程工程研究所 | Reaction device for preparing methyl chlorosilane and reaction system comprising same |
| CN102211770A (en) * | 2010-04-12 | 2011-10-12 | 中国科学院过程工程研究所 | Method for preparing porous silicon material by using catalytic reaction of silicon and halogenated hydrocarbon |
| CN102407168A (en) * | 2011-09-26 | 2012-04-11 | 鲁西化工集团股份有限公司硅化工分公司 | Reusing method for waste contact masses from third stage cyclone separator in methylchlorosilane synthesis |
| CN104151343A (en) * | 2014-07-21 | 2014-11-19 | 鲁西化工集团股份有限公司硅化工分公司 | Additive capable of improving utilization rate of silicon power in synthesis of methyl chlorosilane |
| CN106000429A (en) * | 2016-06-15 | 2016-10-12 | 苏州铜宝锐新材料有限公司 | Catalyst and application thereof |
| CN108043430A (en) * | 2017-12-18 | 2018-05-18 | 苏州铜宝锐新材料有限公司 | Catalyst and its application |
| CN108525614A (en) * | 2018-06-24 | 2018-09-14 | 唐山三友硅业有限责任公司 | Reactor for the experiment of silicon bronze body contacts reactivity worth |
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| JPH09194490A (en) * | 1996-01-12 | 1997-07-29 | Shin Etsu Chem Co Ltd | Production of silanes |
| US6423860B1 (en) * | 2000-09-05 | 2002-07-23 | General Electric Company | Method for promoting dialkyldihalosilane formation during direct method alkylhalosilane production |
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| CN102212080A (en) * | 2010-04-12 | 2011-10-12 | 中国科学院过程工程研究所 | Reaction device for preparing methyl chlorosilane and reaction system comprising same |
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