CN112452304B - Method and equipment for preparing composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan - Google Patents
Method and equipment for preparing composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 90
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 88
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 25
- 239000010703 silicon Substances 0.000 title claims abstract description 25
- 238000011282 treatment Methods 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims description 89
- 239000007788 liquid Substances 0.000 claims description 74
- 238000001556 precipitation Methods 0.000 claims description 36
- 238000006386 neutralization reaction Methods 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 230000007246 mechanism Effects 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 20
- 238000007790 scraping Methods 0.000 claims description 20
- 239000003814 drug Substances 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 15
- 239000002351 wastewater Substances 0.000 claims description 13
- 238000004062 sedimentation Methods 0.000 claims description 11
- 238000004064 recycling Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 claims 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000005429 filling process Methods 0.000 description 6
- 239000002912 waste gas Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000009776 industrial production Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
- B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- B01D53/26—Drying gases or vapours
- B01D53/261—Drying gases or vapours by adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5281—Installations for water purification using chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of chlorosilane raffinate treatment and recovery, in particular to a method and equipment for preparing a composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan.
Description
Technical Field
The invention relates to the technical field of chlorosilane raffinate treatment and recovery, in particular to a method and equipment for preparing a composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan.
Background
Most of domestic polysilicon production processes produce chlorosilane residual liquid, and the main components of the chlorosilane residual liquid are as follows: silicon tetrachloride, dichlorosilane, trichlorosilane and the like have complex components, can generate severe reaction when meeting water and hydrogen and release a large amount of hydrochloric acid and hydrogen, are difficult to recycle, have great influence on the environment, and have become the bottleneck of development of the polysilicon industry due to the fact that the yield of the chlorosilane residual liquid is huge and the chlorosilane residual liquid is scientifically and effectively recycled.
The method for preparing the composite adsorbent by utilizing the chlorosilane raffinate and the chitosan is provided for recycling the chlorosilane raffinate, has high practical value, is characterized in that hydrochloric acid and silicic acid generated by hydrolysis of the chlorosilane are directly utilized, a certain amount of hydrochloric acid is separated, chitosan, glutaraldehyde and the like are added, and the composite adsorbent is subjected to composite modification to obtain the silica-chitosan composite adsorbent with a hydrophobic function.
Therefore, a technical scheme is needed at present to solve the technical problems that no industrial production equipment for preparing the composite adsorbent from the chlorosilane residual liquid and the chitosan is available in industrial production, the treatment efficiency of the chlorosilane residual liquid is low, the treatment effect is poor, and the recycling rate of the chlorosilane residual liquid is affected.
Disclosure of Invention
The invention aims at: aiming at the technical problems that no industrial production equipment for preparing the composite adsorbent by using chlorosilane raffinate and chitosan in industrial production exists at present, the treatment efficiency of the chlorosilane raffinate is low, the treatment effect is poor, and the recycling rate of the chlorosilane raffinate is affected, the method and the equipment for preparing the composite adsorbent by using the chlorosilane raffinate and chitosan are provided.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for preparing the composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan comprises the steps of enabling the chlorosilane raffinate and nitrogen to flow into a stirring chamber of a reaction container along a same material gun, stirring and reacting, quantitatively injecting each reactant into the stirring chamber after independently stirring, introducing compressed air towards an opening of the material gun in the stirring chamber, carrying out gas wrapping reaction to generate adsorbent, enabling the adsorbent to enter a settling chamber of the reaction container in an overflow manner, and enabling the adsorbent in a floating state in the settling chamber to be input into a drying unit from a discharge port on the side wall of the reaction container in the overflow manner.
According to the method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan, the raw materials are filled in a manner of mixing the chlorosilane raffinate and the nitrogen, so that a material gun is not blocked in the feeding process, the accuracy of the feeding amount is ensured, the mixing liquid consisting of the chlorosilane raffinate and each reaction reagent in a reaction container is facilitated to be disturbed, the reaction is promoted, the reaction time is shortened, the uniformity of particles of the prepared adsorbent is improved, the using effect of the prepared adsorbent is improved, meanwhile, the compressed air is further disturbed by adopting a manner of opposite flushing and introducing the compressed air, the material gun is prevented from being blocked by the adsorbent generated by the reaction of the chlorosilane raffinate and each reaction reagent, the reaction time is further shortened, the using effect of the adsorbent is improved, in addition, more bubbles are formed in the mixing liquid due to the introduction of the nitrogen and the compressed air, the adsorbent generated by the wrapping and clamping reaction floats to the surface of the mixing liquid, the prepared adsorbent is conveniently separated in advance in an overflow manner, and the reaction efficiency is further improved.
As a preferable scheme of the invention, the adsorbent in a floating state in the settling chamber enters an overflow groove in the settling chamber in an overflow mode and is output from the discharge port. The adsorbent is output after two overflow treatments, so that the separation effect of the adsorbent in the preparation process is improved, the time and resource consumption for treating chlorosilane residual liquid are reduced, and the treatment efficiency is improved.
As a preferable mode of the invention, the mixed liquid in the precipitation chamber is input into the drying unit after passing through the neutralization precipitation unit, and the neutralization precipitation unit is used for introducing the neutralization agent to react with the mixed liquid. The chlorosilane raffinate treatment process is safer and more environment-friendly, and secondary pollution is avoided.
As a preferable scheme of the invention, the wastewater output by the neutralization and precipitation unit is input into a storage tank for temporary storage and is introduced into a reaction vessel for recycling through a liquid return pipeline. Avoiding secondary pollution caused by wastewater discharge, being beneficial to reducing the filling of water in the reaction process and saving resources.
As a preferred embodiment of the present invention, the gas in the reaction vessel and the neutralization precipitation unit is fed into the exhaust gas treatment unit through an exhaust pipe. Avoiding secondary pollution caused by exhaust emission and ensuring the environmental protection of the chlorosilane residual liquid treatment process to the greatest extent.
As a preferable mode of the invention, the adsorbent in a floating state in the settling chamber is pushed to move towards the discharge port by a scraping mechanism arranged in the reaction vessel. The overflow separation of the adsorbent is obtained through the promotion of the scraping mechanism, and the treatment efficiency of the chlorosilane residual liquid treatment process is improved.
The equipment for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan comprises a raw material supply unit, a reaction container, a neutralization precipitation unit and a drying unit which are communicated through pipelines, wherein the raw material supply unit comprises a chlorosilane raffinate storage tank, a nitrogen storage tank, a compressed gas supply mechanism and a medicament pre-mixing line, the medicament pre-mixing line comprises a plurality of medicament barrels, a stirring chamber and a precipitation chamber are arranged in the reaction container, the reaction container and the neutralization precipitation unit are connected with an exhaust gas treatment unit through an exhaust pipe, and the neutralization precipitation unit is communicated with the reaction container through a liquid return pipeline.
According to the equipment for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan, disclosed by the invention, the equipment production line for the chlorosilane raffinate treatment process is formed by adopting the combination of the raw material supply unit, the reaction container, the neutralization precipitation unit, the drying unit and the waste gas treatment unit, so that the liquid and the gas in the chlorosilane raffinate treatment process are effectively, safely and environmentally-friendly treated, secondary pollution caused in the chlorosilane raffinate treatment process is avoided, and the economic and environmental-friendly utilization of the chlorosilane raffinate is realized.
As a preferable scheme of the invention, the side wall of the reaction vessel is provided with a discharge port, the inside of the reaction vessel corresponding to the discharge port is provided with an overflow groove, and the discharge port is positioned above the liquid level of the mixed liquid in the reaction vessel.
As a preferable scheme of the invention, a scraping mechanism is arranged in the reaction container and comprises a power mechanism and a scraping blade, and the power mechanism drives the scraping blade to move.
As the preferable scheme of the invention, the bottom of the sedimentation chamber and the bottom of the neutralization sedimentation unit are respectively provided with a material collecting tank, the material collecting tank is in a horn shape with a big upper part and a small lower part, and the material collecting tank is communicated with the drying unit through a material discharging pipe.
In summary, by adopting the technical scheme, the method for preparing the composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan has the beneficial effects that:
1. the raw materials are filled in a mode of mixing the chlorosilane residual liquid and the nitrogen, so that a material gun is not blocked in the feeding process, the accuracy of feeding amount is ensured, the mixed liquid consisting of the chlorosilane residual liquid and each reaction medicament in a reaction container is disturbed, the reaction is promoted, the reaction time is reduced, the uniformity of particles of the prepared adsorbent is improved, and the use effect of the adsorbent is improved;
2. by adopting a mode of introducing compressed air in opposite flushing, the compressed air further disturbs the mixed liquid, so that the adsorbent generated by the reaction of chlorosilane residual liquid and each reaction reagent is prevented from blocking a material gun, the reaction time is further shortened, and the use effect is improved;
3. because of the introduction of nitrogen and compressed air, more bubbles are formed in the mixed liquid, and the adsorbent generated by the wrapping reaction floats to the surface of the mixed liquid, the early separation of the prepared adsorbent is conveniently realized in an overflow mode, and the reaction efficiency is further improved;
the device for preparing the composite silicon adsorbent by utilizing the chlorosilane residual liquid and the chitosan has the beneficial effects that:
the equipment production line for the chlorosilane residual liquid treatment process is formed by combining the raw material supply unit, the reaction container, the neutralization and precipitation unit, the drying unit and the waste gas treatment unit, so that the liquid and the gas in the chlorosilane residual liquid treatment process are effectively, safely and environmentally-friendly treated, secondary pollution caused by the chlorosilane residual liquid treatment process is avoided, and the economic and environmentally-friendly utilization of the chlorosilane residual liquid is realized.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing a composite silicon adsorbent using chlorosilane raffinate and chitosan according to the present invention;
FIG. 2 is a schematic structural view of the reaction vessel according to the present invention.
Icon: 1-gun, 2-reaction vessel, 21-stirring chamber, 22-settling chamber, 23-discharge port, 24-overflow tank, 25-collecting tank, 3-scraping mechanism, 4-chlorosilane raffinate storage tank, 5-nitrogen storage tank, 6-compressed gas supply mechanism, 7-neutralization settling unit, 8-drying unit, 9-waste gas treatment unit, 10-medicament barrel, 20-storage tank, 30-liquid return pipeline, 40-exhaust pipe, 50-discharge pipe and 60-stirring mechanism.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1 and 2, in the method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan, the chlorosilane raffinate and the nitrogen flow along the same material gun 1 into a stirring chamber 21 of a reaction vessel 2 to be stirred and reacted, each reactant is quantitatively injected into the stirring chamber 21 after being independently stirred, compressed air is introduced into the stirring chamber 21 by opposite flushing towards an opening of the material gun 1, the gas is entrained and reacted to generate the adsorbent, the adsorbent enters a settling chamber 22 of the reaction vessel 2 in an overflow manner, and the adsorbent in a floating state in the settling chamber 22 is input into a drying unit 8 from a discharge port 23 on the side wall of the reaction vessel 2 in an overflow manner.
According to the method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan, the characteristic that the chlorosilane raffinate is subjected to hydrolysis equilibrium reaction to generate silicon dioxide is combined with the prior art that the silicon dioxide is modified into a modified silicon dioxide adsorbent product with good hydrophobicity by adopting polymerization reaction between the chitosan and glutaraldehyde in the hydrolysis process, the silicon dioxide chitosan composite adsorbent product is prepared, the whole preparation process is combined with each other, reaction heat release and chemical equilibrium are effectively utilized, efficient, energy-saving and environment-friendly preparation of the silicon dioxide chitosan composite adsorbent product is promoted, full recycling of the chlorosilane raffinate is realized, the specific equipment is arranged in the preparation method by combining equipment structures in a targeted manner in a material filling process, a conveying process and a separation process, wherein in the filling process, the raw material filling process is carried out in a manner of adopting mixed flow of the chlorosilane raffinate and nitrogen, a material gun 1 is not blocked in the filling process, the accuracy of the feeding amount is ensured, the mixed liquid consisting of the chlorosilane and each reaction medicament in a reaction container 2 is facilitated to be disturbed, the reaction time is shortened, the uniformity of the adsorbent is promoted, the air flow of the adsorbent is improved, the air flow is improved, the compressed air flow is further reduced, the air flow is further influenced by the compressed air flow is further, and the air flow is compressed by the compressed air is further, and the air flow is more influenced by the compressed air flow is further formed by the compressed by the air in the air gun, and the air flow is compressed by the compressed particles, the adsorbent generated by the wrapping reaction floats to the surface of the mixed liquid, so that the prepared adsorbent can be conveniently separated in advance in an overflow mode in the separation process, the reaction efficiency is further improved, and the use effect of the adsorbent is improved.
Specifically, a plurality of stirring mechanisms 60 are arranged in the stirring chamber 21 of the reaction vessel 2, the stirring mechanisms 60 comprise a motor, a rotating rod and blades arranged on the rotating rod, mixed raw materials consisting of chlorosilane residual liquid and nitrogen, which are input by the material gun 1, enter the stirring chamber 21 and then are fully mixed and stirred by the stirring mechanisms 60, the mixed raw materials fully react with each reaction reagent added into the stirring chamber 21, the prepared adsorbent is wrapped by bubbles under the disturbance of the nitrogen and compressed air, and the adsorbent floats to the surface of the mixed liquid easily, so that the mixed raw materials can be conveniently input into the settling chamber 22 of the reaction vessel 2 from the stirring chamber 21 of the reaction vessel 2 in an overflow mode.
Preferably, the adsorbent in a floating state in the settling chamber 22 enters the overflow trough 24 in the settling chamber 22 in an overflow manner and is output from the discharge port 23.
Specifically, the adsorbent is input into the precipitation chamber 22 from the stirring chamber 21 of the reaction vessel 2 to finish the first overflow treatment, and is input into the overflow groove 24 from the precipitation chamber 22 to finish the second overflow treatment, so that the two overflow treatments of the adsorbent are realized, the treatment time and the resource consumption for separating the adsorbent from the mixed liquid are reduced, the separation efficiency of the adsorbent in the preparation process is improved, and the treatment efficiency of the chlorosilane raffinate is improved.
Preferably, the mixed liquid in the precipitation chamber 22 is fed into the drying unit 8 after passing through the neutralization precipitation unit 7, and the neutralization precipitation unit 7 is used for introducing the neutralizing agent to react with the mixed liquid.
Specifically, the wastewater generated by the reaction of the chlorosilane residual liquid and the chitosan also contains more non-separated adsorbents, and the direct discharge of the wastewater can cause environmental pollution, the wastewater after the twice overflow treatment in the reaction vessel 2 is input into the neutralization precipitation unit 7, alkali liquor and PAM are introduced, the wastewater treatment is realized, the generation of the adsorbents is further promoted, the full recycling of the chlorosilane residual liquid is realized, the chlorosilane residual liquid treatment process is safer and more environment-friendly, and the secondary pollution is avoided.
Preferably, the wastewater output by the neutralization precipitation unit 7 is input into the storage tank 20 for temporary storage and is introduced into the reaction vessel 2 through the liquid return pipeline 30 for recycling.
Specifically, the wastewater treated by the neutralization precipitation unit 7 flows back into the reaction vessel 2, so that on one hand, chlorosilane residual liquid and chitosan and other medicaments continuously react, the chlorosilane residual liquid is fully recovered, on the other hand, secondary pollution caused by wastewater discharge is avoided, the filling of water in the reaction process is reduced, and resources are saved.
Preferably, the gases in the reaction vessel 2 and the neutralization precipitation unit 7 are fed into the exhaust gas treatment unit 9 via an exhaust pipe 40.
Specifically, the exhaust gas treatment unit 9 is a tail gas treatment device such as a conventional spray tower, so as to ensure the environmental protection of the chlorosilane residual liquid treatment process to the greatest extent.
Preferably, the adsorbent in a floating state in the settling chamber 22 is pushed to move toward the discharge port 23 by the scraping mechanism 3 provided in the reaction vessel 2.
Specifically, the scraping mechanism 3 is manufactured in a manner of driving the scraping blade to move by power, the scraping mechanism 3 is used for promoting overflow separation of the adsorbent, and the treatment efficiency of the chlorosilane residual liquid treatment process is improved.
Example 2
As shown in fig. 1 and 2, the apparatus for preparing a composite silicon adsorbent using chlorosilane raffinate and chitosan of the present embodiment comprises a raw material supply unit, a reaction vessel 2, a neutralization precipitation unit 7 and a drying unit 8 which are communicated through pipes, wherein the raw material supply unit comprises a chlorosilane raffinate tank 4, a nitrogen tank 5, a compressed gas supply mechanism 6 and a chemical pre-mixing line, the chemical pre-mixing line comprises a plurality of chemical tanks 10, the reaction vessel 2 and the neutralization precipitation unit 7 are connected with an exhaust gas treatment unit 9 through an exhaust pipe 40, and the neutralization precipitation unit 7 is communicated with the reaction vessel 2 through a liquid return pipe 30.
The equipment for preparing the composite silicon adsorbent by utilizing the chlorosilane residual liquid and the chitosan of the embodiment combines the raw material supply unit, the reaction vessel 2, the neutralization precipitation unit 7, the drying unit 8 and the waste gas treatment unit 9 to form an equipment production line for the chlorosilane residual liquid treatment process, so that liquid, gas and waste water in the chlorosilane residual liquid treatment process are effectively, safely and environmentally treated, secondary pollution caused by the chlorosilane residual liquid treatment process is avoided, and economic and environmental utilization of the chlorosilane residual liquid is realized.
Specifically, each medicament barrel 10 of the medicament pre-mixing line corresponds to contain a medicament, each medicament barrel 10 is internally provided with a stirring mechanism 60 and a mechanical diaphragm pump, the medicament barrels 10 are communicated with a water supply main through pipelines, each medicament is respectively subjected to automatic concentration accurate adjustment and then is supplied with power by the mechanical diaphragm pump to be input into the reaction container 2 for use, the precision and automation of the medicament filling process are realized, and the medicament filling process can be controlled by a PLC system in the prior art.
Preferably, a discharge hole 23 is formed in the side wall of the reaction vessel 2, an overflow groove 24 is formed in the reaction vessel 2 corresponding to the discharge hole 23, the discharge hole 23 is located above the liquid level of the mixed liquid in the reaction vessel 2, a material collecting groove 25 is formed in the bottom of the settling chamber 22 and the bottom of the neutralization settling unit 7, the material collecting groove 25 is in a horn shape with a large upper part and a small lower part, and the material collecting groove 25 is communicated with the drying unit 8 through a material discharging pipe 50.
Specifically, the stirring chamber 21 and the sedimentation chamber 22 which are communicated at a position close to the top of the reaction vessel 2 are formed in the reaction vessel 2 by a partition plate which is obliquely arranged, the chlorosilane raffinate storage tank 4 inputs the chlorosilane raffinate into the stirring chamber 21 through the material gun 1, the nitrogen storage tank 5 inputs nitrogen into the material gun, the chlorosilane raffinate and the nitrogen enter the stirring chamber 21 to fully react with other reaction reagents added into the stirring chamber 21, then the generated adsorbent enters the sedimentation chamber 22 in an overflow manner under the disturbance of compressed air input by the compressed air supply mechanism 6, an overflow groove 24 is arranged on the inner side wall of the sedimentation chamber 22, a collecting groove 25 is arranged at the bottom, the adsorbent floating on the liquid surface in the sedimentation chamber 22 enters the overflow groove 24 in an overflow manner and is output from the discharge hole 23, the precipitated adsorbent enters the collecting groove 25 to be collected in a concentrated manner and then is output from the bottom discharge pipe 50, and the liquid separated from the sedimentation chamber 22 is input into the neutralization sedimentation unit 7 through a pipeline for further treatment.
Preferably, a scraping mechanism 3 is arranged in the reaction container 2, the scraping mechanism 3 comprises a power mechanism and a scraping blade, and the power mechanism drives the scraping blade to move. Preferably, the power mechanism is a rotary structure formed by a fluted disc and a chain, drives a scraping blade arranged on the chain to move, pushes the adsorbent in a suspended state to enter the sedimentation chamber 22 from the stirring chamber 21 and then enter the overflow groove 24, and promotes separation of the adsorbent.
Specifically, neutralization precipitation unit 7 includes the box and sets up a plurality of baffles in the box, adjacent baffle dislocation set forms the overflow channel, set up the filter media that is used for stopping the adsorbent and pass through in the overflow channel, make the adsorbent deposit to the aggregate tank 25 of bottom after being stopped, simultaneously, set up the baffle and separate overflow channel input one side into a plurality of cavities, adjacent cavity top and bottom intercommunication correspond through pipe connection a medicament bucket 10 and set up rabbling mechanism 60 in every cavity, in order to promote the going on of reaction, realize the make full use of to chlorosilane raffinate, and avoid the secondary pollution that reaction waste water caused.
Specifically, the overflow channel output side is provided with the level gauge for detect the liquid level in neutralization precipitation unit 7, when the liquid level is too high or in the reaction vessel liquid concentration be less than 20%, introduce waste water cyclic utilization in the reaction vessel 2 through liquid return pipeline 30, avoid the waste water overflow that the liquid level is too high to guarantee the smooth going on of reaction process, realize chlorosilane raffinate treatment process's feature of environmental protection.
Further, the adsorbents outputted from the reaction vessel 2 and the neutralization precipitation unit 7 are uniformly inputted into the drying unit 8 for drying treatment to obtain a composite adsorbent with extremely fine particles, large specific surface area and good use effect, preferably the drying unit is a spray drying system, that is, the aqueous adsorbent is sprayed into the drying unit 8 in a spray state through a spray nozzle for drying treatment of drying and press filtration, so that the drying efficiency and the product quality of the prepared adsorbent are improved.
Specifically, the dried adsorbent is separated from hot air by the cyclone dust collector, so that the efficient separation of the adsorbent is realized, the concentrated collection and treatment of waste gas are facilitated, the residual quantity of the adsorbent in the waste gas is reduced, the adsorption efficiency is improved, and the risk of secondary pollution is reduced.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. The method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan is characterized in that the chlorosilane raffinate and the nitrogen flow along the same material gun (1) into a stirring chamber (21) of a reaction container (2) to be stirred and reacted, each reactant is quantitatively injected into the stirring chamber (21) after being independently stirred, compressed air is introduced into the stirring chamber (21) towards an opening of the material gun (1) in a counter-flushing way, the adsorbent generated by gas-carrying reaction enters a settling chamber (22) of the reaction container (2) in an overflow way, and the adsorbent in a floating state in the settling chamber (22) is input into a drying unit (8) from a side wall discharge hole (23) of the reaction container (2) in an overflow way.
2. The method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan according to claim 1, wherein the adsorbent in a floating state in the settling chamber (22) enters an overflow groove (24) in the settling chamber (22) in an overflow manner and is output from the discharge port (23).
3. The method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan according to claim 2, wherein the mixed liquid in the precipitation chamber (22) is input into the drying unit (8) after passing through the neutralization precipitation unit (7), and the neutralization precipitation unit (7) is used for introducing a neutralizing agent to react with the mixed liquid.
4. The method for preparing the composite silicon adsorbent by utilizing the chlorosilane raffinate and the chitosan as claimed in claim 3, wherein the wastewater output by the neutralization and precipitation unit (7) is input into a storage tank (20) for temporary storage and is introduced into a reaction vessel (2) for recycling through a liquid return pipeline (30).
5. A method for preparing a composite silicon adsorbent using chlorosilane raffinate and chitosan as claimed in claim 3 wherein the gases in the reaction vessel (2) and the neutralisation precipitation unit (7) are fed into the exhaust gas treatment unit (9) via an exhaust pipe (40).
6. The method for preparing a composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan according to claim 1, wherein the adsorbent in a floating state in the precipitation chamber (22) is pushed to move towards the discharge port (23) by a scraping mechanism (3) arranged in the reaction vessel (2).
7. Utilize chlorosilane raffinate and chitosan preparation composite silicon adsorbent's equipment, its characterized in that includes raw materials supply unit, reaction vessel (2), neutralization precipitation unit (7) and drying unit (8) through the pipeline intercommunication, raw materials supply unit includes chlorosilane raffinate storage tank (4), nitrogen gas storage tank (5), compressed gas supply mechanism (6) and medicament pre-mix line, medicament pre-mix line includes a plurality of medicament barrels (10), be provided with teeter chamber (21) and settling chamber (22) in reaction vessel (2), reaction vessel (2) with neutralization precipitation unit (7) are connected with exhaust-gas treatment unit (9) through blast pipe (40), neutralization precipitation unit (7) pass through return liquid pipeline (30) with reaction vessel (2) intercommunication.
8. The device for preparing the composite silicon adsorbent by utilizing the chlorosilane residual liquid and the chitosan according to claim 7, wherein a discharge port (23) is arranged on the side wall of the reaction vessel (2), an overflow groove (24) is arranged in the reaction vessel (2) corresponding to the discharge port (23), and the discharge port (23) is positioned above the liquid level of the mixed liquid in the reaction vessel (2).
9. The device for preparing the composite silicon adsorbent by utilizing the chlorosilane residual liquid and the chitosan, as claimed in claim 8, wherein a scraping mechanism (3) is arranged in the reaction container (2), the scraping mechanism (3) comprises a power mechanism and a scraping blade, and the power mechanism drives the scraping blade to move.
10. The equipment for preparing the composite silicon adsorbent by utilizing the chlorosilane residual liquid and the chitosan according to claim 9, wherein a material collecting groove (25) is formed in the bottom of the sedimentation chamber (22) and the bottom of the neutralization sedimentation unit (7), the material collecting groove (25) is in a horn shape with a big top and a small bottom, and the material collecting groove (25) is communicated with the drying unit (8) through a material discharging pipe (50).
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