CN114478610A - Production process of vinyl silane - Google Patents
Production process of vinyl silane Download PDFInfo
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- CN114478610A CN114478610A CN202210082986.6A CN202210082986A CN114478610A CN 114478610 A CN114478610 A CN 114478610A CN 202210082986 A CN202210082986 A CN 202210082986A CN 114478610 A CN114478610 A CN 114478610A
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- acetylene
- silane
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- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 182
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 182
- 239000002904 solvent Substances 0.000 claims abstract description 56
- 238000000746 purification Methods 0.000 claims abstract description 54
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910000077 silane Inorganic materials 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002893 slag Substances 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 31
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical group [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 22
- 239000000920 calcium hydroxide Substances 0.000 claims description 22
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 21
- 239000005997 Calcium carbide Substances 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 19
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 12
- 239000010865 sewage Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 230000007246 mechanism Effects 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000002608 ionic liquid Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims 3
- 239000000203 mixture Substances 0.000 claims 2
- 239000002244 precipitate Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract 2
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 30
- 230000000694 effects Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000002699 waste material Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0805—Compounds with Si-C or Si-Si linkages comprising only Si, C or H atoms
Abstract
The utility model provides a production technology of vinyl silane, relate to vinyl silane production technical field, production technology includes two processes, in the preparation process of acetylene, acetylene that acetylene generator continuous production is after drying device is dried, get into gas purification device from the air inlet, acetylene after the purification is let in alkali wash tank by gas purification device's gas outlet again and is fully contacted with alkali lye, in the reaction process of acetylene and silane, at first, be full of carrier solvent in the packed tower, secondly, let in silane and acetylene to the packed tower, silane and acetylene in the packed tower get into reation kettle after reacting for a certain time, reation kettle's liquid outlet passes through the circulating pump and carries the product to the knockout tower in, carrier solvent gets into in the solvent recovery jar from the knockout tower, vinyl silane crude gets into in the crude receiving tank after the condenser condensation from the knockout tower. On the basis of ensuring the sufficient reaction, two raw materials are simultaneously introduced in a specific mode, so that the time required by the reaction is shortened, and the reaction efficiency is improved.
Description
Technical Field
The invention relates to the technical field of vinyl silane production, in particular to a production process of vinyl silane.
Background
In the chemical production process of vinyl silane which is often used as a coupling agent, the raw materials for producing the vinyl silane are silane and acetylene, at present, a tower type reaction is mostly adopted, a reaction solvent and the raw materials are added into a kettle at one time and then the acetylene is introduced for slow reaction, and the product is transferred to the next procedure until the raw materials are completely consumed, and the method has the defects that: silane in the tower is difficult to be quickly loaded on a solvent in the early stage, so that the silane is difficult to be fully reacted with acetylene, and the acetylene needs to be continuously introduced for a long time, so that the single reaction time is as long as a plurality of hours, the time is long, and the reaction efficiency is low.
Acetylene as a raw material for production is generally produced from calcium carbide. Pure acetylene is colorless and odorless gas, and acetylene generated from calcium carbide often has special unpleasant odor due to the mixing of impurities such as hydrogen sulfide, phosphine, arsine and the like, so that the acetylene gas needs to be purified in industrial application to obtain pure acetylene gas for industrial production.
In the prior art, the processes for purifying crude acetylene gas mainly comprise two processes: sodium hypochlorite purification process and concentrated sulfuric acid purification process.
The sulfuric acid purification process has its limitations, and concentrated sulfuric acid absorbs water in acetylene gas and gives off dilution heat. When the temperature of the 98 percent sulfuric acid rises to be higher than 18 ℃, the speed of acetylene decomposition is greatly accelerated, and the temperature of the solution rises quickly, so that great potential safety hazards exist.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a production process of vinyl silane, which comprises the following specific scheme:
a production process of vinyl silane comprises a preparation process of acetylene and a reaction process of acetylene and silane;
in the preparation process of acetylene, acetylene continuously produced by an acetylene generator is dried by a drying device, enters a gas purification device from a gas inlet, is sequentially introduced into different acid liquor from the gas purification device to fully contact with the acetylene to purify the acetylene, the purified acetylene is introduced into an alkali washing tank from a gas outlet of the gas purification device to fully contact with alkali liquor, and the acetylene after alkali washing is secondarily introduced into the drying device to obtain neutral, impurity-free and dry acetylene;
in the reaction process of acetylene and silane, firstly, a carrier solvent which does not participate in the reaction is filled in a packed tower and then is kept for a certain time, then silane is continuously introduced from the top of the packed tower, silane is introduced into the packed tower at three different flow rates of a flow rate A, a flow rate B and a flow rate C within ten minutes to half an hour, neutral, impurity-free and dry acetylene is continuously introduced from different positions of the packed tower during the introduction of the silane, the silane and the acetylene in the packed tower enter a reaction kettle to react for a certain time, a product is conveyed into a separation tower from a liquid outlet of the reaction kettle through a circulating pump, the carrier solvent and a crude vinyl silane product are separated in the separation tower, the carrier solvent enters a solvent recovery tank from the separation tower, and the crude vinyl silane product enters a crude product receiving tank from the separation tower after being condensed by a condenser.
Further, in the preparation process of acetylene, the acid solution introduced into the gas purification device comprises concentrated sulfuric acid with different mass fractions, wherein the mass fractions are 80%, 96% and 85%.
Further, the concentrated sulfuric acid that gas purification device corresponds different mass fractions is including the purification tank that a plurality of intercommunications set up, be equipped with air inlet, the gas outlet that advances from top to bottom on the purification tank, acetylene passes through the air inlet and gets into first purification tank after, gets into the air inlet of next purification tank from the gas outlet, sets gradually, and wherein, the dwell time of acetylene in every purification tank is five to ten minutes.
Further, a stirring mechanism is arranged in the purification tank, and when acetylene is initially in the purification tank, the stirring mechanism is started to rotate at a rotating speed of 30r/min until the acetylene leaves the purification tank.
Further, before acetylene produced by an acetylene generator enters a drying device, the acetylene is physically washed in a circulating washer to remove carbide slag attached to the acetylene, then the washed acetylene is introduced into an ionic liquid purification tower to remove chemical impurities in the acetylene, then the purified acetylene sequentially passes through a condenser and a gas-water separator to obtain crude acetylene, and the crude acetylene enters the drying device.
Further, in the process of producing acetylene by the acetylene generator, the sewage generated by the acetylene generator is calcium hydroxide slag slurry, the calcium hydroxide slag slurry is discharged into a sewage sedimentation tank, the sewage sedimentation tank stands for a certain time, then upper clear water is pumped out, the sediment calcium carbide slag slurry is transferred to a grinding machine for primary grinding, the particle size of the ground calcium carbide slag slurry is controlled to be less than 30um, then the calcium carbide slag slurry is diluted and introduced into a suspension separator for separation to obtain calcium hydroxide slurry with the calcium hydroxide content of more than 98%, and the calcium hydroxide slurry is subjected to vacuum dehydration to form calcium carbide slag.
Further, the flow rate a is greater than the flow rate B, the flow rate B is less than the flow rate C, and the flow rate C is less than or equal to the flow rate a.
Furthermore, in the reaction process of acetylene and silane, the carrier solvent in the solvent recovery tank enters the packed tower and the reaction kettle again through the solvent delivery pump for recycling.
Further, in the reaction process of acetylene and silane, a carrier solvent of a solvent delivery pump firstly enters a venturi mixer, the venturi mixer simultaneously carries out gas-liquid mixing on the acetylene and the carrier solvent in the venturi mixer through the treated acetylene, and the acetylene and the carrier solvent are respectively introduced into a packed tower and a reaction kettle from a liquid outlet of the venturi mixer after mixing.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, acetylene is obtained in real time through the acetylene preparation process without wasting manpower and physically storing acetylene, and after the acetylene obtained in the preparation process is sequentially treated by the drying device, the acid liquid, the alkali liquid and the drying device, odorous impurities in the acetylene are removed, and the acetylene gas which is free of moisture and is neutral and stable is obtained. And then, the reaction process of acetylene and silane is carried out, wherein silane and acetylene enter a packed tower for a certain time, specifically, silane is introduced into the packed tower in a mode of different flow rates, acetylene is introduced into the packed tower from different positions of the packed tower, so that the silane is firstly uniformly dispersed in a carrier volume and gradually reacts with the acetylene within ten minutes to half an hour, and the silane is smoothly combined with the acetylene in the downward moving process by utilizing the height direction of the packed tower.
(2) The acetylene is positioned in front of the gas purification device, water is removed by the drying device, the acetylene is assisted by the acid liquor with the smallest concentration for drying, the water absorption effect is achieved, even the concentrated sulfuric acid can release heat at the moment, the harm is small, on the premise that the acid liquor is fully contacted with the acetylene by stirring the acid liquor by the stirring mechanism, the purification effect of the acetylene during purification by the subsequent acid liquor with higher concentration is the best, and finally, the acetylene is secondarily purified by the acid liquor with smaller concentration, so that the purification effect is further improved, and the acid liquor with higher concentration can be degraded to be recycled as the next acid liquor with lower concentration, so that the material cost is reduced;
(3) the acetylene generator can recover waste of the generated calcium hydroxide slag slurry while producing acetylene, and prepare multipurpose carbide slag after grinding, diluting, separating and vacuum dehydrating, wherein the carbide slag can be used for replacing limestone to prepare cement, producing quicklime as a carbide raw material, producing light bricks and the like, and accords with the concept of energy conservation;
(4) through setting up the venturi mixer, earlier load the acetylene in the carrier solvent after the recovery, after the carrier solvent of load acetylene lets in the filled tower again, with the carrier solvent in the filled tower originally in the load silane's mode opposite for the silane in the carrier solvent, the acetylene can combine with faster speed, need not to wait that the acetylene combines with the carrier solvent again after getting into the filled tower, lead to the waste of time, thereby improve reaction efficiency.
Drawings
FIG. 1 is a block diagram of an overall architecture of an embodiment of the present invention;
FIG. 2 is a flow chart showing the operation between the acetylene generator and the drying apparatus according to the present invention;
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1 and 2, a process for producing vinyl silane includes a preparation process of acetylene and a reaction process of acetylene and silane.
In the preparation process of acetylene, acetylene continuously produced by an acetylene generator is dried by a drying device, enters a gas purification device from a gas inlet, is sequentially introduced into different acid liquids by the gas purification device to be fully contacted with the acetylene, the introduced acid liquids comprise concentrated sulfuric acid with different mass fractions of 80%, 96% and 85%, the acetylene is purified, the purified acetylene is introduced into an alkali washing tank from a gas outlet of the gas purification device to be fully contacted with alkali liquor, and the acetylene after alkali washing is secondarily introduced into the drying device to obtain neutral, impurity-free and dry acetylene.
The concentrated sulfuric acid that gas purification device corresponds different quality fractions is including the purifying tank that a plurality of intercommunications set up, is equipped with air inlet, the gas outlet of advancing the upper and lower play on the purifying tank, and acetylene passes through the air inlet and gets into first purifying tank after, gets into the air inlet of next purifying tank from the gas outlet, sets gradually, and wherein, the dwell time of acetylene in every purifying tank is five to ten minutes, guarantees fully to contact between acetylene and the purifying tank. And a stirring mechanism is arranged in the purification tank, and when acetylene is initially positioned in the purification tank, the stirring mechanism is started automatically and rotates at the rotating speed of 30r/min until the acetylene leaves the purification tank. In the step, the acetylene after drying is firstly assisted by the acid liquor with the minimum concentration for drying, so that the water absorption effect is achieved, even if concentrated sulfuric acid can release heat at the moment, the harm is small, on the premise that the acid liquor is fully contacted with the acetylene by stirring the acid liquor by the stirring mechanism, the purification effect of the acetylene is the best when the acetylene is purified by the subsequent acid liquor with the high concentration, and finally, the acetylene is secondarily purified by the acid liquor with the small concentration, so that the purification effect is further improved.
Preferably, before acetylene produced by the acetylene generator enters the drying device, the acetylene is physically washed in a circulating washer, acetylene slag attached to the acetylene is removed, the washed acetylene is introduced into an ionic liquid purification tower to remove chemical impurities in the acetylene, the purified acetylene sequentially passes through a condenser and a gas-water separator to obtain crude acetylene, and the crude acetylene enters the drying device. By the steps, carbide slag in the acetylene which is just prepared is washed away, the temperature of the acetylene is reduced, impurities such as sulfur, phosphorus and arsenic in the acetylene are removed under the action of the ionic liquid purifying tower, and subsequent drying, purifying and drying processes can be normally carried out after most of the impurities in the acetylene are removed.
Preferably, in the process of producing acetylene by the acetylene generator, the sewage generated by the acetylene generator is calcium hydroxide slag slurry, the calcium hydroxide slag slurry is discharged into a sewage sedimentation tank, the sewage sedimentation tank stands for a certain time, then upper clear water is pumped out, the sediment calcium carbide slag slurry is transferred to a grinding machine for primary grinding, the particle size of the ground calcium carbide slag slurry is controlled to be less than 30um, then the calcium carbide slag slurry is diluted and introduced into a suspension separator for separation to obtain calcium hydroxide slurry with the calcium hydroxide content of more than 98%, and the calcium hydroxide slurry is subjected to vacuum dehydration to form calcium carbide slag. Through the step, the generated calcium hydroxide slag slurry can be subjected to waste recovery, and the multipurpose carbide slag is prepared through grinding, dilution, separation and vacuum dehydration.
After acetylene is prepared, the reaction process of acetylene and silane is carried out, firstly, a carrier solvent which does not participate in the reaction is filled in a packed tower and is kept for a certain time, secondly, silane is continuously introduced into the packed tower from the top of the packed tower, silane is introduced into the packed tower at three different flow rates of a flow rate A, a flow rate B and a flow rate C within ten minutes to half an hour, the flow rate A is greater than the flow rate B, the flow rate B is less than the flow rate C, and the flow rate C is less than or equal to the flow rate A. During silane introduction, continuously introducing neutral, impurity-free and dry acetylene from different positions of a packed tower, after silane and acetylene in the packed tower enter a reaction kettle to react for a certain time, conveying a product to a separation tower through a liquid outlet of the reaction kettle by a circulating pump, separating a carrier solvent and a crude vinyl silane product in the separation tower, introducing the carrier solvent into a solvent recovery tank from the separation tower, and condensing the crude vinyl silane product from the separation tower by a condenser and then introducing the crude vinyl silane product into a crude product receiving tank.
In the reaction process of acetylene and silane, the carrier solvent in the solvent recovery tank enters the packed tower and the reaction kettle again through the solvent delivery pump for recycling, it needs to be noted that the carrier solvent of the solvent delivery pump enters the venturi mixer first, the venturi mixer simultaneously carries out gas-liquid mixing with the carrier solvent in the venturi mixer through the processed acetylene, and the acetylene and the carrier solvent are respectively introduced into the packed tower and the reaction kettle through a liquid outlet of the venturi mixer after mixing. In the step, acetylene is loaded in the carrier solvent recovered by the solvent recovery tank, and after the carrier solvent loaded with acetylene is introduced into the packed tower again, the method is opposite to the method for loading silane in the original carrier solvent in the packed tower, so that the silane and the acetylene in the carrier solvent can be combined at a higher speed, the acetylene does not need to be combined with the carrier solvent after entering the packed tower, the time waste is caused, and the reaction efficiency is improved.
Accordingly, the present invention proposes example 1.
Example 1
A process for preparing vinyl silane includes such steps as generating acetylene by acetylene generator, physically washing acetylene by cyclic washer, removing acetylene dregs, introducing the washed acetylene to ionic liquid tower to remove chemical impurities, passing the purified acetylene through condenser and gas-water separator to obtain coarse acetylene, and drying. After being dried by a drying device, the acetylene gas enters a gas purification device from a gas inlet, the acetylene gas sequentially passes through purification tanks filled with concentrated sulfuric acid with the mass fractions of 80%, 96% and 85% by the gas purification device, the concentrated sulfuric acid is fully contacted with acetylene in the purification tanks, wherein the residence time of the acetylene in each purification tank is eight minutes, and when the acetylene is initially in the purification tanks, a stirring mechanism in the purification tanks is started to rotate at the rotating speed of 30r/min until the acetylene leaves the purification tanks. And then, introducing the acetylene purified by the concentrated sulfuric acid into an alkaline washing tank from an air outlet of the gas purification device to fully contact with the alkaline solution, and introducing the acetylene after alkaline washing into a drying device for the second time to obtain neutral, impurity-free and dry acetylene.
When the acetylene generator produces acetylene, the produced sewage is calcium hydroxide slag slurry, the calcium hydroxide slag slurry is discharged into a sewage sedimentation tank, after the sewage sedimentation tank is stood for a certain time, clear water on the upper layer is pumped out, the sediment calcium carbide slag slurry is transferred to a grinding machine for primary grinding, the particle size of the ground calcium carbide slag slurry is controlled to be less than 30 mu m, then the calcium carbide slag slurry is diluted, the calcium carbide slag slurry is introduced into a suspension separator for separation to obtain the calcium hydroxide slurry with the calcium hydroxide content of more than 98%, and the calcium hydroxide slurry is subjected to vacuum dehydration to form the calcium carbide slag. After acetylene is prepared, the reaction process of acetylene and silane is carried out, firstly, a carrier solvent which does not participate in the reaction is filled in a packed tower and then is kept for fifteen minutes, secondly, silane is continuously introduced from the top of the packed tower, silane is introduced into the packed tower within twenty minutes at three different flow rates of a flow rate A, a flow rate B and a flow rate C, the flow rate A is greater than the flow rate B, the flow rate B is less than the flow rate C, and the flow rate C is less than or equal to the flow rate A. During the silane feeding period, continuously feeding neutral, impurity-free and dry acetylene from different positions of a packed tower, after the silane and the acetylene in the packed tower enter a reaction kettle for reaction for two hours, conveying a product into a separation tower through a liquid outlet of the reaction kettle by a circulating pump, separating a carrier solvent and a vinyl silane crude product in the separation tower, feeding the carrier solvent into a solvent recovery tank from the separation tower, feeding the carrier solvent in the solvent recovery tank into a venturi mixer through a solvent conveying pump, mixing the carrier solvent with the acetylene in the venturi mixer in a gas-liquid manner, respectively feeding the mixed carrier solvent into the packed tower and the reaction kettle to re-enter the packed tower and the reaction kettle for recycling, and condensing the vinyl silane crude product from the separation tower through a condenser and then feeding the vinyl silane crude product into a crude product receiving tank.
So far, the preparation of the crude product of the vinyl silane is finished, and the next procedure can be carried out. For the crude vinylsilane prepared in example 1, the yield of vinylsilane was found to be 95.4%.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (9)
1. The production process of the vinyl silane is characterized by comprising the steps of preparing acetylene and reacting the acetylene with silane;
in the preparation process of acetylene, acetylene continuously produced by an acetylene generator is dried by a drying device, enters a gas purification device from a gas inlet, is sequentially introduced into different acid liquor from the gas purification device to fully contact with the acetylene to purify the acetylene, the purified acetylene is introduced into an alkali washing tank from a gas outlet of the gas purification device to fully contact with alkali liquor, and the acetylene after alkali washing is secondarily introduced into the drying device to obtain neutral, impurity-free and dry acetylene;
in the reaction process of acetylene and silane, firstly, a carrier solvent which does not participate in the reaction is filled in a packed tower and then is kept for a certain time, then silane is continuously introduced from the top of the packed tower, silane is introduced into the packed tower at three different flow rates of a flow rate A, a flow rate B and a flow rate C within ten minutes to half an hour, neutral, impurity-free and dry acetylene is continuously introduced from different positions of the packed tower during the introduction of the silane, the silane and the acetylene in the packed tower enter a reaction kettle to react for a certain time, a product is conveyed into a separation tower from a liquid outlet of the reaction kettle through a circulating pump, the carrier solvent and a crude vinyl silane product are separated in the separation tower, the carrier solvent enters a solvent recovery tank from the separation tower, and the crude vinyl silane product enters a crude product receiving tank from the separation tower after being condensed by a condenser.
2. The process for producing vinylsilane according to claim 1, wherein in the step of producing acetylene, the acid solution introduced into the gas purification apparatus comprises concentrated sulfuric acids with different mass fractions, wherein the mass fractions are 80%, 96% and 85%.
3. The vinyl silane production process according to claim 2, wherein the gas purification device comprises a plurality of purification tanks which are arranged in a communicated manner and correspond to concentrated sulfuric acid with different mass fractions, the purification tanks are provided with a gas inlet and a gas outlet, the acetylene enters the first purification tank through the gas inlet and then enters the gas inlet of the next purification tank through the gas outlet, and the acetylene is sequentially arranged, wherein the residence time of the acetylene in each purification tank is five to ten minutes.
4. The process for producing vinylsilane according to claim 3, wherein said purge tank is provided with a stirring mechanism, and when acetylene is initially in the purge tank, the stirring mechanism is automatically started to rotate at a rotation speed of 30r/min until acetylene leaves the purge tank.
5. The process for producing vinylsilane according to claim 1, wherein acetylene produced by the acetylene generator is physically washed in a circulating washer before entering the drying device to remove carbide slag attached to acetylene, then the washed acetylene is introduced into an ionic liquid purification tower to remove chemical impurities in the acetylene, and then the purified acetylene passes through a condenser and a gas-water separator in sequence to obtain crude acetylene, and the crude acetylene enters the drying device.
6. The process for producing vinylsilane according to claim 1, wherein in the process of producing acetylene by the acetylene generator, the sewage generated by the acetylene generator is calcium hydroxide slag slurry, the calcium hydroxide slag slurry is discharged into a sewage sedimentation tank, the sewage sedimentation tank is kept still for a certain time, then the upper clear water is pumped out, the precipitate calcium carbide slag slurry is transferred to a grinder for primary grinding, the particle size of the ground calcium carbide slag slurry is controlled to be less than 30um, then the calcium carbide slag slurry is diluted and introduced into a suspension separator for separation to obtain the calcium hydroxide slurry with the calcium hydroxide content of more than 98%, and the calcium hydroxide slurry is subjected to vacuum dehydration to form calcium carbide slag.
7. The process for producing vinylsilane according to claim 1, wherein the flow rate a is greater than the flow rate B, the flow rate B is less than the flow rate C, and the flow rate C is less than or equal to the flow rate a.
8. The process for producing vinylsilane according to claim 1, wherein the carrier solvent in the solvent recovery tank is recycled by being re-introduced into the packed tower or the reaction kettle by the solvent delivery pump in the reaction process of acetylene and silane.
9. A process for preparing vinyl silane as claimed in claim 8, wherein in the reaction step of acetylene and silane, the carrier solvent of solvent delivery pump is first introduced into Venturi mixer, the Venturi mixer passes through the treated acetylene simultaneously, the acetylene and the carrier solvent are mixed in Venturi mixer to form gas-liquid mixture, and the mixture is introduced into packed tower and reaction kettle from the liquid outlet of Venturi mixer.
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| CN202210082986.6A CN114478610A (en) | 2022-01-25 | 2022-01-25 | Production process of vinyl silane |
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| CN202210082986.6A CN114478610A (en) | 2022-01-25 | 2022-01-25 | Production process of vinyl silane |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967968A (en) * | 2016-07-01 | 2016-09-28 | 北京神雾环境能源科技集团股份有限公司 | Acetylene purification system and method |
| CN111004267A (en) * | 2019-12-13 | 2020-04-14 | 杭州崇耀科技发展有限公司 | Preparation method of hexamethyldisiloxane |
| CN113861233A (en) * | 2021-10-27 | 2021-12-31 | 湖北兴瑞硅材料有限公司 | Preparation process and device of methyltrimethoxysilane |
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- 2022-01-25 CN CN202210082986.6A patent/CN114478610A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967968A (en) * | 2016-07-01 | 2016-09-28 | 北京神雾环境能源科技集团股份有限公司 | Acetylene purification system and method |
| CN111004267A (en) * | 2019-12-13 | 2020-04-14 | 杭州崇耀科技发展有限公司 | Preparation method of hexamethyldisiloxane |
| CN113861233A (en) * | 2021-10-27 | 2021-12-31 | 湖北兴瑞硅材料有限公司 | Preparation process and device of methyltrimethoxysilane |
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