CN1343670A - Process and system for synthesizing organosilicon monomer by direct method - Google Patents
Process and system for synthesizing organosilicon monomer by direct method Download PDFInfo
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- CN1343670A CN1343670A CN 01136583 CN01136583A CN1343670A CN 1343670 A CN1343670 A CN 1343670A CN 01136583 CN01136583 CN 01136583 CN 01136583 A CN01136583 A CN 01136583A CN 1343670 A CN1343670 A CN 1343670A
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Abstract
A process for synthetizing organosilicon monomer by direct method includes mixing silcion powder with mixed catalyst powder in liquid-phase ultrasonic mixer to uniformly disperse the catalyst power on the surface of silicon particles (100 micron of granularity), removing solvent, and reaction with chloronated hydrocarbon gas is fluidized-bed reactor. Its advantages include high reaction speed, and less consumption of catalyst.
Description
Technical field
The present invention relates to a kind of chemical industry synthetic technology, particularly a kind of processing method and system that utilizes the direct method synthesizing organosilicon monomer.
Background technology
At present, direct method synthesizing organosilicon monomer technology is to feed chlorinated hydrocarbon gas to make silica flour and powdery mixed catalyst (comprising Primary Catalysts that contains Red copper oxide or cuprous chloride and the promotor of being made up of other metals) fluidisation in fluidized-bed, finish the catalyzed chemical reaction of silica flour and chlorinated hydrocarbon (as methyl chloride or mono chloro benzene) gas, generate organosilane monomer (as dichlorodimethylsilane or chloro-phenyl-silane).
Owing to powdery mixed catalyst in the reaction process contacts the bad activity of such catalysts that is difficult to give full play to silica flour, and fluidisation such as takes out of at reason, need during with this technology continuous production when adding the raw material silica flour, constantly to append the powdery mixed catalyst, just can keep this catalyzed reaction and normally carry out.As described in USP5596119 (1997), the add-on of powdery mixed catalyst is about 5% of a silica flour feeding quantity.
As everyone knows, Gu the reaction that chlorinated hydrocarbon and silica flour carry out under the effect of powdery mixed catalyst is the gas-solid-catalyzed reaction of a complexity.Solid-state silica flour carries out solid-solid reaction with solid-state powdery mixed catalyst earlier in the reaction process, and (η is Cu mutually to generate copper-silicon alloy at the surface in contact of silicon and copper containing catalyst
3Si).Siliciumatom in this copper-silicon alloy has than high reaction activity, has constituted main reaction in this reaction system thereby can be under the certain reaction temperature generate organosilane monomer with gas phase chlorination hydrocarbon direct reaction.Fail to contact the powdery mixed catalyst that forms copper-silicon alloy with silicon under temperature of reaction, wherein contained copper is called free copper.It has advantages of high catalytic activity to the cracking of gas phase chlorination hydrocarbon.The chlorinated hydrocarbon cracking obtains H
2, C, HCl etc. do not wish the product wanted.The chlorinated hydrocarbon scission reaction is the main side reaction of this reaction system.For quickening main reaction, face upward only side reaction and must optimize reaction conditions (temperature, pressure, gas speed etc.), screening silica flour (foreign matter content, granularity etc.), screening powdery mixed catalyst (chemical composition compatibility, crystal formation, granularity etc.).As USP4504596, USP4503165, USP4450282, USP4487950 is described, and Red copper oxide that filters out at present or cuprous chloride catalyst are all very thin, and particle diameter is below 3 microns.Have agglomeration in these fine powders under surface action power, the size of coacervate is about about 20 microns.Silica flour and powdery mixed catalyst carry out drying and mixing at one in nitrogen fluidizing fluidized-bed in the existing technology, and coacervate is difficult to be disperseed under this fluidization conditions.The existence of coacervate has hindered silicon and copper tight the contact and the formation of copper-silicon alloy also causes having a large amount of free copper in the reaction system, produces more side reaction.
Summary of the invention
The purpose of this invention is to provide a kind of new process that utilizes the direct method synthesizing organosilicon monomer, carry out having introduced liquid phase before fluidisation mixing and the exsiccant operation at silica flour and powdery mixed catalyst, in liquid phase, introduce ultrasonic energy to realize the dispersion of powdered catalyst coacervate, it can closely be contacted with silica flour.The silica flour particle diameter is 50 to 150 microns, under the ultrasonic energy effect, the micron order powdery mixed catalyst of reuniting in the liquid phase can be disperseed and the part covers silicon powder surface, the surface in contact that has enlarged silicon and copper is long-pending, thereby is that the add-on that reduces the powdery mixed catalyst in the production process has significantly been created condition.
This technology and system thereof are achieved by the following technical solution:
A kind of synthesis technique system of direct method synthesizing organosilicon monomer, this system comprises silica flour storage tank, powdery mixed catalyst storage tank, nitrogen fluidized bed dryer, compound storage tank, fluidized-bed reactor and corresponding connecting tube, it is characterized in that having set up in this technology a solvent cycle and utilize system, this system by solvent tank, the dispersion that makes the powdery mixed catalyst and silica flour can mixed uniformly ultrasonic mixer, solvent cycle pump, condenser, the desolventizing jar that removes the mixture solvent by pipe connection together; Ultrasonic mixer inlet set in this technology links to each other with three storage tanks by pipeline, and outlet links to each other with the desolventizing jar; The outlet of set desolventizing jar links to each other with pipeline with fluidized bed dryer, and the desolventizing jar also links to each other with solvent cycle pump, condenser by pipeline respectively.
A kind of method that adopts above-mentioned synthesis technique, this processing method is carried out successively as follows:
A. silica flour, powdery mixed catalyst and solvent are at room temperature mixed by solvent tank, silica flour storage tank, powdery mixed catalyst storage tank inflow ultrasonic mixer respectively, become suspension by the mixed material of ultrasonic mixer, the suspension solid holdup is controlled at 20～50%;
B. the suspension after supersound process enters the desolventizing jar, in the desolventizing jar, pass through the most of solvent of solvent cycle pump suction strainer with filter-tipped suction pipe earlier, through steam jacket the compound in the jar is heated to boiling point to remove residual solvent then, sloughs that solvent should be less than 1% in the compound of solvent;
C. the compound of sloughing solvent enters the nitrogen fluidized bed dryer again and carries out drying treatment;
D. the compound after the drying treatment enters the compound storage tank, enters in the fluidized-bed reactor and reacts.
In above-mentioned synthesis technique, used solvent is methyl chloride, methylene dichloride, trichloromethane, dilute hydrochloric acid, monochloroethane or its mixture.Used ultrasonic mixer ultrasonic power density range is 10 watts/liter～500 watts/liter, and ultrasonic frequency range is 0.1MHz～200MHz, and the mixing speed scope is 10 rev/mins～300 rev/mins.
In the above-mentioned synthesis technique system, set ultrasonic mixer mainly comprises motor, shaft coupling, colvent inlet, powder inlet, powder mixier main body, stir shaft, discharge gate etc., the axle center that it is characterized in that ultrasonic mixer is equipped with screw blade, and the ultrasonic mixer wall is equipped with ultrasonic launching head.
In the above-mentioned synthesis technique system, set desolventizing jar mainly comprises compound inlet, solvent vapo(u)r outlet, heating steam inlet, desolventizing can body, discharge port, condensation-water drain, the suction pipe of being with filtering head is equipped with in the axle center that it is characterized in that the desolventizing jar, take solvent by suction pipe away by the solvent cycle pump, the desolventizing tank skin is provided with the heating jacket that makes remaining liquid phase medium vaporization.
In the above-mentioned synthesis technique system, solvent, powdery mixed catalyst and an amount of silica flour can also be added ultrasonic mixer, utilize ultrasonic wave and mechanical stirring that the powdery mixed catalyst is pre-dispersed.Add silica flour then, under ultrasonic and mechanical stirring condition with pre-dispersed good mixed catalyst and silica flour thorough mixing.
Can reduce the add-on of powdery mixed catalyst by the improved technology of the present invention, thereby reduce production costs, reduce the pollution of copper, and can also reduce the side reaction in the reaction system environment.
Description of drawings
Fig. 1 is technical process of the present invention and structural representation.
Fig. 2 is a ultrasonic mixer structural representation of the present invention.
Fig. 3 is a desolventizing jar structure synoptic diagram of the present invention.
Embodiment
Specify technical process of the present invention and concrete implementation step below in conjunction with accompanying drawing:
Synthesis technique of the present invention system mainly is made up of solvent tank 1, silica flour storage tank 2, powdery mixed catalyst storage tank 3, product outlet 4, ultrasonic mixer 5, solvent cycle pump 6, fluidized-bed reactor 7, condenser 8, desolventizing jar 9, fluidized bed dryer 10, compound storage tank 12 and corresponding connecting tube.Annexation between each equipment is as follows: solvent tank 1, ultrasonic mixer 5, solvent cycle pump 6, condenser 8, remove the desolventizing jar 9 of mixture solvent, and form solvent cycle by pipe connection together and utilized system; The ultrasonic mixer inlet links to each other with storage tank 1,2,3 by pipeline, and outlet links to each other with desolventizing jar 9; Desolventizing jar 9, its outlet links to each other with pipeline with fluidized bed dryer, and the desolventizing jar also links to each other with pipeline with solvent cycle pump, condenser respectively.Fluidized bed dryer 10 inlets link to each other with 9 outlets of desolventizing jar with pipeline, and the bottom is provided with nitrogen inlet 13, and links to each other by the top of pipeline with compound storage tank 12.The outlet of compound storage tank 12 is linked to each other by pipeline with the bottom of fluidized-bed reactor 7, and the bottom of fluidized-bed reactor 7 is provided with chlorinated hydrocarbon gas inlet 11, and top is provided with product and exported for 4 (as shown in Figure 1).
The concrete implementation step of this technology is as follows:
Silica flour, powdery mixed catalyst and solvent at room temperature flow into ultrasonic mixer 5 by solvent tank 1, silica flour storage tank 2, powdery mixed catalyst storage tank 3 respectively to be mixed, and solvent, silica flour and mixed catalyst three's weight ratio is 3: 1: 0.02.The silica flour particle diameter is the 50-100 micron, and purity is 98%.Solvent adopts compatible with chemical reaction system and silicon face is had the liquid of certain cleanup action, can adopt trichloromethane, monochloroethane, chlorobenzene, hydrochloric acid or their mixture.The powdery mixed catalyst adopts two kinds of powdered catalysts comprising that powdery mixed catalyst that cuprous chloride and promotor constitute and Red copper oxide and promotor constitute.Have mechanical stirring arm to make powder-material form suspension in the ultrasonic mixer, the suspension solid holdup is controlled at 20%-50%.The ultrasonic mixer wall is equipped with several ultrasonic launching heads, and ultrasonic power density is controlled at 10 watts/liter-500 watts/liter in the mixing tank.Ultrasonic suspension was controlled at 5 minutes-10 minutes action time, can adopts periodical operation also can adopt operate continuously.
Solution after the supersound process enters desolventizing jar 9, in the desolventizing jar, take solvent with filter-tipped suction pipe away by solvent cycle pump 6 earlier, through steam jacket the compound in the jar is heated to boiling point then, make solvent gasification after condenser 8 condensations to remove residual solvent.Slough that solvent should be less than 1% in the compound of solvent.The compound of sloughing solvent enters 130-200 ℃ nitrogen fluidized bed dryer 10 again and carries out drying treatment, and the fluidized gas superficial gas velocity is 0.01 meter per second-0.25 meter per second, is controlled at time of drying 30 minutes-3 hours.Compound after drying is handled enters compound storage tank 12, adds in batches or continuously in the fluidized-bed reactor 7 and reacts, and the fluidized-bed reaction actuator temperature is controlled at 280 ℃-300 ℃, and superficial gas velocity is controlled to be 0.15 meter per second.
Accompanying drawing 2 is a ultrasonic mixer structural representation of the present invention.Ultrasonic mixer is made up of mixing tank tank body, spiral stirring system, ultrasonic wave generation systems etc.Mainly comprise motor 1, shaft coupling 2, the support of bearing 3, colvent inlet 4, powder inlet 5, powder mixier main body 6, stir shaft 7, screw blade 8, ultrasonic launching head 9, discharge gate 10 etc., screw blade 8 is installed on the axle center of ultrasonic mixer, and ultrasonic launching head 9 is arranged on the wall of ultrasonic mixer.In the operating process, earlier solvent, powdery mixed catalyst and an amount of silica flour are added ultrasonic mixer, utilize ultrasonic wave and mechanical stirring that the powdery mixed catalyst is pre-dispersed.Add silica flour then, under ultrasonic and mechanical stirring condition with pre-dispersed good mixed catalyst and silica flour thorough mixing.Thereby realize that the fine mixed catalyst that monodispersity is good is evenly attached to the silicon powder particle surface.The silica flour contact that removes solvent and obtain after super-dry promptly can be used for the organosilane monomer building-up reactions.Utilize ultrasonic mixer of the present invention, also solvent, silica flour and powdery mixed catalyst can be added together, under ultrasonic and churned mechanically effect, make the dispersion of catalyzer and be achieved simultaneously with the uniform mixing of silica flour.Apparatus of the present invention both can adopt the intermittent mode operation, also can adopt the continuous mode operation.
Adopt the active direct synthesization of dimethyl dichlorosilane of cuprous chloride CuCl catalyzer (DDS) organosilane monomer, silica flour, powdery mixed catalyst are stored in basin 2 and 3 respectively.The silica flour particle diameter is 50 to 150 microns, and purity is 98%.The component of active cuprous chloride catalyst system is as shown in table 1.
Table 1. cuprous chloride catalyst system is formed
| Title | Apparent particle size/micron | Weight fraction/% |
| Active CuCl | ????1-20 | ????90 |
| | ????1-5 | ????9 |
| | ????1-5 | ????1 |
Select for use trichloromethane to make solvent, be stored in solvent tank under the room temperature.Solvent, powdery mixed catalyst and an amount of silica flour added ultrasonic mixer pre-dispersed 10 minutes together, added residue silica flour remix then and disperseed 10 minutes.Solvent, silica flour and mixed catalyst three's weight ratio is 3: 1: 0.02.The ultrasonic power density of ultrasonic mixer is 50 watts/liter, and frequency is 10MHz, and mixing speed is 50 rev/mins.Desolventizing jar temperature is controlled at 100 ℃.The trichloromethane solvent vapo(u)r that trichloromethane solvent that filtration pump is extracted out and desolventizing jar steam reclaims to be stored in the solvent tank through condensation and recycles.
Slough that solvent is controlled at below 1% in the compound of solvent, this material enters 180 ℃ nitrogen fluidized-bed again and makes drying treatment, be controlled at time of drying about 1 hour, compound changes the compound basin over to then, is added in batches or continuously to carry out building-up reactions in the fluidized-bed reactor again.The fluidized-bed reaction actuator temperature is controlled at 280 ℃ to 300 ℃, and superficial gas velocity is controlled at 0.15 meter per second.The compound of handling with the present invention carries out building-up reactions in fluidized-bed reactor, the rate of catalysis reaction of silica flour still remain on 3% weight (silicon)/hour, the selectivity that generates DDS still remains on more than 80%, and the add-on of powdery mixed catalyst is reduced to 2% of silica flour add-on.The catalyzer add-on only is 2/5ths of existing process catalyst add-on 5%.
Adopt the copper oxide catalyst system, raw material is identical with embodiment 1 with synthetic reaction condition, direct method synthesization of dimethyl dichlorosilane (DDS) organosilane monomer.The component of active copper oxide catalyst system is as shown in table 2.Table 2. copper oxide catalyst system is formed
| Title | Apparent particle size/micron | Weight fraction/% |
| Cupric oxide | ????1-20 | ????90 |
| | ????1-5 | ????9 |
| | ????1-5 | ????1 |
Select for use methyl chloride to make solvent.Solvent, silica flour and powdery mixed catalyst add ultrasonic mixer together, and three's weight ratio is 3: 1: 0.02.Mixture stopped in ultrasonic mixer 15 minutes, and ultrasonic power is 50 watts/liter, and frequency is 10MHz, 50 rev/mins of mixing speed.Desolventizing process and drying process are identical with embodiment 1.In fluidized-bed reactor, carry out building-up reactions with technology of the present invention, the rate of catalysis reaction of silica flour still can reach 3% weight (silicon)/hour, the selectivity that generates DDS is still more than 80%, and the add-on of powdery mixed catalyst is reduced to 2% of silica flour add-on.The catalyzer add-on only is 2/5ths of existing process catalyst add-on 5%.
Claims (7)
1. the synthesis technique system of a direct method synthesizing organosilicon monomer, this system comprises silica flour storage tank [2], powdery mixed catalyst storage tank [3], nitrogen fluidized bed dryer [10], compound storage tank [12], fluidized-bed reactor [7] and corresponding connecting tube, it is characterized in that having set up in this technology a solvent cycle and utilize system, this system is by solvent tank [1], make the dispersion and the silica flour energy mixed uniformly ultrasonic mixer [5] of powdery mixed catalyst, solvent cycle pump [6], condenser [8], the desolventizing jar [9] that removes the mixture solvent passes through pipe connection together: described ultrasonic mixer inlet is by pipeline and storage tank [1], [2], [3] link to each other, outlet links to each other with the desolventizing jar; The outlet of described desolventizing jar links to each other with pipeline with fluidized bed dryer, and the desolventizing jar also links to each other with pipeline with solvent cycle pump, condenser respectively.
2. according to the described synthesis technique of claim 1 system, described ultrasonic mixer [5] mainly comprises motor [1], shaft coupling [2], colvent inlet [4], powder inlet [5], powder mixier main body [6], stir shaft [7], discharge gate [10] etc., the axle center that it is characterized in that ultrasonic mixer is equipped with screw blade [8], and the ultrasonic mixer wall is equipped with ultrasonic launching head [9].
3. according to the described synthesis technique of claim 1 system, described desolventizing jar [9] mainly comprises compound inlet [1], solvent vapo(u)r outlet [2], heating steam inlet [3], desolventizing can body [4], discharge port [9], condensation-water drain [10], the suction pipe of being with filtering head [8] is equipped with in the axle center that it is characterized in that desolventizing jar [9], and the desolventizing tank skin is equipped with the heating jacket [7] that makes remaining liquid phase medium vaporization.
4. one kind is adopted synthetic process as claimed in claim 1, and this processing method is carried out successively as follows:
A. silica flour, powdery mixed catalyst and solvent are at room temperature mixed by solvent tank [1], silica flour storage tank [2], powdery mixed catalyst storage tank [3] inflow ultrasonic mixer [5] respectively, become suspension by the mixed material of ultrasonic mixer, the suspension solid holdup is controlled at 20%～50%;
B. the suspension after supersound process enters desolventizing jar [9], in the desolventizing jar, remove most of solvent with solvent cycle pump [6] by the filtering head suction strainer earlier, through steam jacket the compound in the jar is heated to boiling point to remove residual solvent then, sloughs that solvent should be less than 1% in the compound of solvent;
C. the compound of sloughing solvent enters nitrogen fluidized bed dryer [10] again and carries out drying treatment;
D. the compound after the drying treatment enters compound storage tank [12], enters in the fluidized-bed reactor [7] to react again.
5. according to the described synthetic process of claim 4, it is characterized in that the solvent described in the synthesis technique is methyl chloride, methylene dichloride, trichloromethane, dilute hydrochloric acid, monochloroethane or its mixture.
6. according to claim 4 or 5 described synthetic process, it is characterized in that described ultrasonic mixer ultrasonic power density range is 10 watts/liter～500 watts/liter, ultrasonic frequency range is 0.1MHz～200MHz, and the mixing speed scope is 10 rev/mins～300 rev/mins.
7. according to the described synthetic process of claim 4, it is characterized in that in a step, solvent, powdery mixed catalyst and an amount of silica flour being added ultrasonic mixer, utilize ultrasonic wave and mechanical stirring that the powdery mixed catalyst is pre-dispersed, add the residue silica flour then, will pre-dispersed good mixed catalyst under ultrasonic and mechanical stirring condition with remain the silica flour thorough mixing.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404131C (en) * | 2005-08-17 | 2008-07-23 | 中国石油天然气股份有限公司 | Method for preparing silicon-copper touch body in use for synthesizing organic chlorsilane |
| CN101579613B (en) * | 2008-04-08 | 2013-08-14 | 中国石油化工股份有限公司 | Agglomerate removal device |
| CN104624120A (en) * | 2015-02-12 | 2015-05-20 | 东至绿洲环保化工有限公司 | Organic silicon heating bath synthesis device |
| CN104645902A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Organic silicon synthetic fluidized bed with hot runner device |
| CN104645886A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Vulcanization bed for synthesizing organic silicon |
| CN104645901A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Fluidizer capable of producing organic silicon |
| CN104645884A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Thermal synthesis device of organic silicon |
| CN104689761A (en) * | 2015-02-12 | 2015-06-10 | 东至绿洲环保化工有限公司 | Organic silicon synthesizing equipment with solar device |
| CN104707538A (en) * | 2015-02-12 | 2015-06-17 | 东至绿洲环保化工有限公司 | Pneumatic organic silicon synthesis device |
| CN104801241A (en) * | 2015-02-12 | 2015-07-29 | 东至绿洲环保化工有限公司 | Organosilicon production fluidized bed |
| CN109821482A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
-
2001
- 2001-10-19 CN CNB011365838A patent/CN1157397C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404131C (en) * | 2005-08-17 | 2008-07-23 | 中国石油天然气股份有限公司 | Method for preparing silicon-copper touch body in use for synthesizing organic chlorsilane |
| CN101579613B (en) * | 2008-04-08 | 2013-08-14 | 中国石油化工股份有限公司 | Agglomerate removal device |
| CN104624120A (en) * | 2015-02-12 | 2015-05-20 | 东至绿洲环保化工有限公司 | Organic silicon heating bath synthesis device |
| CN104645902A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Organic silicon synthetic fluidized bed with hot runner device |
| CN104645886A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Vulcanization bed for synthesizing organic silicon |
| CN104645901A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Fluidizer capable of producing organic silicon |
| CN104645884A (en) * | 2015-02-12 | 2015-05-27 | 东至绿洲环保化工有限公司 | Thermal synthesis device of organic silicon |
| CN104689761A (en) * | 2015-02-12 | 2015-06-10 | 东至绿洲环保化工有限公司 | Organic silicon synthesizing equipment with solar device |
| CN104707538A (en) * | 2015-02-12 | 2015-06-17 | 东至绿洲环保化工有限公司 | Pneumatic organic silicon synthesis device |
| CN104801241A (en) * | 2015-02-12 | 2015-07-29 | 东至绿洲环保化工有限公司 | Organosilicon production fluidized bed |
| CN109821482A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
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