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CN108607267A - A kind of recovery processing technique and its processing unit of organosilicon slag slurry - Google Patents

A kind of recovery processing technique and its processing unit of organosilicon slag slurry Download PDF

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Publication number
CN108607267A
CN108607267A CN201810448036.4A CN201810448036A CN108607267A CN 108607267 A CN108607267 A CN 108607267A CN 201810448036 A CN201810448036 A CN 201810448036A CN 108607267 A CN108607267 A CN 108607267A
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China
Prior art keywords
slag slurry
gas
organosilicon slag
evaporator
organosilicon
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CN201810448036.4A
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Chinese (zh)
Inventor
羊实
周旭
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Chengdu Sili Kang Polytron Technologies Inc
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Chengdu Sili Kang Polytron Technologies Inc
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Priority to CN201810448036.4A priority Critical patent/CN108607267A/en
Publication of CN108607267A publication Critical patent/CN108607267A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D50/00Combinations of methods or devices for separating particles from gases or vapours
    • B01D50/20Combinations of devices covered by groups B01D45/00 and B01D46/00

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The present invention discloses a kind of recovery processing technique and its processing unit of organosilicon slag slurry, technique includes following operating procedure, including following operating procedure, (1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature is to 26-28 DEG C, it is stirred with 30-40r/min of low-speed mixer, stirs 20-30min, collect tetramethylsilane gas;(2) 30-40 DEG C are then heated to, with the rotating speed of 20-30r/min, 1h-2h is stirred, collects the gas trichlorosilane gas of generation;(3) continue to be heated to 75-77 DEG C, with the rotating speed of 30-40r/min, stir 1.5h-2h, collect the gas tetrachloromethane gas of generation;(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, carry out solid-liquor separation.Low-boiling point material tetramethylsilane, trichlorosilane, the tetrachloromethane in organosilicon slag slurry are detached it according to boiling point by adjusting the temperature of evaporator in the technical program, the substance after separation carries out classification recycling.

Description

A kind of recovery processing technique and its processing unit of organosilicon slag slurry
Technical field
The present invention relates to the treatment technologies of silicon slurry, and in particular to a kind of recovery processing technique of organosilicon slag slurry and its place Manage device.
Background technology
Organosilicon slag slurry is generated waste in organic silicon monomer building-up process, accounts for about monomer yield 3%.It is main The responseless silica flour of fluid bed, copper powder, the zinc powder taken out of by high-boiling components and on a small quantity form, and high-boiling components refer to methylchlorosilane list 80-215 DEG C of the boiling range generated in body building-up process, containing silicon-silicon key, carbon-carbon-silicon key, silicon-oxygen-silicon structure two Silane mixture.It exposes easy firing in air and forms smog, it is necessary to carry out Harmless processing.
Currently, manufacturing enterprise is to be recycled high-boiling components therein by detaching mostly to the processing method of slurry, separation is high Slurry after boiling object, which is directly discharged into water, to be hydrolyzed, because containing part high-boiling components, a large amount of acid mists hydrolyzed to form in slurry, it is necessary into The processing of row Harmless.Manufacturing enterprise is by detaching high-boiling components recycling therein, dividing mostly to the processing method of slurry at present It is hydrolyzed in directly being drained from the slurry after high-boiling components.Because containing part high-boiling components in slurry, a large amount of acid mists hydrolyzed to form are easy It is excessive, cause the pollution to environment.
Based on this, studies and develop and design a kind of recovery processing technique and its processing unit of organosilicon slag slurry.
Invention content
The present invention provides a kind of recovery processing technique of organosilicon slag slurry, this discarded for existing organosilicon slag slurry Object, present in processing procedure the problem of environmental pollution, the technical program is used and is preheated in evaporator, at heating Reason, the high waste in organosilicon slag slurry is separated and recovered according to its boiling point, avoids directly arranging containing the slurry in high-boiling components It is put into water, generates acid mist and cause to change environmental pollution.
The present invention is achieved through the following technical solutions:
A kind of recovery processing technique of organosilicon slag slurry, including following operating procedure:
(1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature uses stirring at low speed to 26-28 DEG C Machine 30-40r/min stirrings, stir 20-30min, collect tetramethylsilane gas;
(2) 30-40 DEG C are then heated to, with the rotating speed of 20-30r/min, 1h-2h is stirred, collects the trichlorine hydrogen of generation Silicon gas;
(3) continue to be heated to 75-77 DEG C, with the rotating speed of 30-40r/min, stir 1.5h-2h, collect the tetrachloro of generation Methane gas;
(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, it is solid to carry out liquid Separation.
Organosilicon slag slurry in the technical program is generated waste in organic silicon monomer building-up process, accounts for about monomer Yield 3%.Its responseless silica flour of fluid bed, copper powder, zinc powder for mainly being taken out of by high-boiling components and on a small quantity form, and high-boiling components are Refer to 80-215 DEG C of the boiling range generated in methyl chlorosilane monomer building-up process, contains silicon-silicon key, carbon-carbon-silicon key, silicon- The disilane mixture of oxygen-silicon structure.It exposes easy firing in air and forms smog, it is necessary to carry out Harmless processing.
And the main waste in organosilicon slag slurry is tetramethylsilane, trichlorosilane, tetrachloromethane, therefore, according to useless The boiling point of gurry, is detached, wherein the boiling point of tetramethylsilane is 26-28 DEG C, and the boiling point of trichlorosilane is 31.8 DEG C, the boiling point of tetrachloromethane is 76.8 DEG C, and heating is evaporated in evaporator, these substances are detached, after separation Organosilicon slag is passed through buck, obtains graininess hydrolysate, carries out solid-liquor separation.
Due to detaching the substance contained in organosilicon slag slurry in the technical program, using the side of this classification processing Method is handled according to the property of substance to be separated, can be reached to the efficiently separating of substance, be cleaned, and avoid organosilicon slag Slurry using during prior art processing method, can avoid part high-boiling components, a large amount of acid mists hydrolyzed to form be easy it is excessive, to ring Border pollutes.
Further, in order to preferably realize the present invention, to the gas of collection in the step (1), step (2), step (3) Then body is collected by filtering.Organosilicon slag slurry forms gas during ebuillition of heated, and gas can carry in evaporation process Some impurity, since the property of due-in collection gas is different, it is therefore desirable to carry out removing miscellaneous operation to gas.
Further, in order to preferably realize the present invention, after being evaporated gas in the step (4), by organosilicon slag slurry It is transferred in solid-liquid separator, buck is passed into the speed of 8m/s -9m/s in solid-liquid separator by high-pressure hydraulic pump, is had Copper powder reaction in machine silicon slurry generates Kocide SD flocky precipitate, is passed through to plate and frame type filter-press, hydrogen-oxygen is isolated in press filtration Change copper, gained alkalinity clear liquid is delivered to next treatment process and uses.
By will be passed into buck and divided after the processing of the organosilicon slag slurry of above-mentioned processing in the technical program From, the copper powder in organosilicon slag slurry to be separated, the method for separation is to react to generate Kocide SD flocky precipitate with buck, Then Kocide SD flocky precipitate is subjected to press filtration separation, the liquid after separation is sent to being handled in next step.
Further, in order to preferably realize the present invention, the buck is sodium hydroxide or potassium hydroxide solution.
Another object of the present invention is to:A kind of organosilicon slag slurry recycling and processing device, including evaporator, evaporator are provided Lower end periphery for hollow cylinder structure, evaporator is provided with sheathed heater, and the inner upper end of evaporator is equipped with filter plate, The upper end of filter plate is equipped with partition board, and cavity is equipped between partition board and filter plate, folded sheet is equipped in cavity;Upper end of evaporator is also Equipped with getter pipe, the input end of getter pipe is in horn-like, and the input end of getter pipe is located at partition board and filter plate is formed by sky Intracavitary, and the input end end face of getter pipe is equipped with filter screen, the aperture of filter screen is 0.1-0.3um, and getter pipe extends to evaporation Connect with four-way valve outside device, three of four-way valve export respectively with first gas collection device, second gas collection device, the Three gas collectors connect.
Organosilicon slag slurry described in the technical program is recycled liquid, is primarily directed to above-mentioned recovery processing technique The device of middle application, evaporator can by the low-boiling-point substances such as tetramethylsilane, trichlorosilane, tetrachloromethane in organosilicon slag slurry into Row separation, and there are certain toxicity, corrosion properties for these low-boiling-point substances, it are detached respectively, then according to corresponding type Property carries out classification processing.
Further, the outlet end of the evaporator is connect with solid-liquid separator, solid-liquid separator and plate and frame type filter-press Connection.
Further, one end of the folded sheet is fixed on the inner wall of evaporator, the other end of folded sheet be fixed on every On plate, and folded sheet is in continuous Z-shaped.
Further, the first gas collection device, second gas collection device, third gas collection device are identical Structure.
Further, the filter plate is to bend to interior arcuation, and the radian of bending is 40-60 °.
Further, the four-way valve is solenoid valve.
Compared with prior art, the present invention having the following advantages and advantages:
(1) it is detached according to the property of low-boiling-point substance in organosilicon slag slurry in the technical program, and by the substance after separation Classification processing is carried out, solves in the prior art directly to set the high-boiling components in organosilicon slag slurry and is hydrolyzed, easy tos produce acid Mist causes environmental pollution.
(2) to low-boiling point material tetramethylsilane, trichlorosilane, the tetrachloromethane in organosilicon slag slurry in the technical program It is detached according to boiling point by adjusting the temperature of evaporator, the substance after separation carries out classification recycling.
(3) recycling and processing device designed also directed to the treatment process of organosilicon slag slurry in the technical program, the device It is simple in structure, it can effectively be recycled according to technique, reduce the influence to environment.
Description of the drawings
Fig. 1 is the structural diagram of the present invention;
Wherein, 1-evaporator, 2-sheathed heaters, 3-filter plates, 4-folded sheets, 5-getter pipes, 6-partition boards, 7-four-way valves, 8-first gas collection devices, 9-second gas collection devices, 10-third gas collection devices.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment, the present invention is made Further to be described in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this The restriction of invention.
Embodiment 1:
A kind of recovery processing technique of organosilicon slag slurry, including following operating procedure:
(1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature uses low-speed mixer to 26 DEG C 30r/min is stirred, and stirs 20min, collects tetramethylsilane gas;
(2) 30 DEG C are then heated to, with the rotating speed of 20r/min, 1h is stirred, collects the gas trichlorosilane gas of generation;
(3) continue to be heated to 75 DEG C, with the rotating speed of 30r/min, stir 1.5h, collect the gas tetrachloromethane gas of generation Body;
(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, it is solid to carry out liquid Separation.
Embodiment 2:
A kind of recovery processing technique of organosilicon slag slurry, including following operating procedure:
(1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature uses low-speed mixer to 28 DEG C 40r/min is stirred, and stirs 30min, collects tetramethylsilane gas;
(2) 40 DEG C are then heated to, with the rotating speed of 30r/min, 2h is stirred, collects the gas trichlorosilane gas of generation;
(3) continue to be heated to 77 DEG C, with the rotating speed of 40r/min, stir 2h, collect the gas tetrachloromethane gas of generation;
(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, it is solid to carry out liquid Separation.
Wherein, after being evaporated gas in the step (4), organosilicon slag slurry is transferred in solid-liquid separator, height is passed through Buck is passed into the speed of 8m/s -9m/s in solid-liquid separator by water pump, and the copper powder reaction in organosilicon slag slurry generates hydrogen Copper oxide flocky precipitate is passed through to plate and frame type filter-press, and Kocide SD is isolated in press filtration, and gained alkalinity clear liquid is delivered to next Treatment process uses.
Embodiment 3:
A kind of recovery processing technique of organosilicon slag slurry, including following operating procedure:
(1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature uses low-speed mixer to 27 DEG C 35r/min is stirred, and stirs 25min, collects tetramethylsilane gas;
(2) 35 DEG C are then heated to, with the rotating speed of 25r/min, 1.5h is stirred, collects the gas trichlorosilane gas of generation Body;
(3) continue to be heated to 76 DEG C, with the rotating speed of 35r/min, stir 2h, collect the gas tetrachloromethane gas of generation;
(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, it is solid to carry out liquid Separation.
Wherein, the buck is sodium hydroxide or potassium hydroxide solution.
Embodiment 4:
As shown in Figure 1, a kind of organosilicon slag slurry recycling and processing device, including evaporator 1, evaporator 1 are hollow cylinder The lower end periphery of structure, evaporator 1 is provided with sheathed heater 2, and the inner upper end of evaporator 1 is equipped with filter plate 3, filter plate 3 Upper end be equipped with partition board 6, cavity is equipped between partition board 6 and filter plate 3, folded sheet 4 is equipped in cavity;The upper end of evaporator 1 is also Equipped with getter pipe 5, the input end of getter pipe 5 is in horn-like, and the input end of getter pipe 5 is located at partition board 6 and 3 shapes of filter plate At cavity in, and the input end end face of getter pipe 5 is equipped with filter screen, and the aperture of filter screen is 0.1-0.3um, and getter pipe 5 prolongs The outside of evaporator 1 is reached to connect with four-way valve 7, three of four-way valve 7 export respectively with first gas collection device 8, the second gas Body collection device 9, third gas collection device 10 connect.
Organosilicon slag slurry is transported in evaporator 1 first in the present embodiment, the temperature in evaporator 1 mainly passes through chuck Heater 2 is adjusted its temperature, and controls its temperature, and the gas being evaporated in the temperature is made to be recycled.
The concrete structure of evaporator 1 is hollow cylinder structure in the present embodiment, therefore this body structure and its principle are ability Well known to field technique personnel, no longer it is described in detail.When being heated to the organosilicon slag slurry liquid in evaporator 1, with temperature Increase, corresponding low-boiling-point substance is evaporated out, the gas being evaporated first by filter plate 3 enter filter plate 3 and partition board 6 it Between cavity in, filter plate 3 is equipped with many filtering apertures here, and aperture is generally 0.5-4.5um, and gas passes through filter plate 3 Can have the effect of centainly tentatively filtering.After gas enters cavity, the folded sheet 4 of setting, the shape of folded sheet 4 are in cavity Rugosity, therefore under the barrier effect of the folded sheet 4, certain barrier effect can be played to the flow direction for collecting gas, allowed It is flowed according to predetermined glide path, and specifically, collecting gas can flow towards the inlet of getter pipe 5.
The arrival end of getter pipe 5 also is located in cavity in the present embodiment, is collected gas and is carried out getter pipe 5, and passes through four Port valve 7 enters in corresponding gas collector, such as first gas collection device 8 or second gas collection device 9 or third Gas collector 10.
To corresponding gas collector, then 7 valve switch of corresponding four-way valve is opened.
Wherein, the gas access end of getter pipe 5 is equipped with filter screen, and the effect of filter screen is the filtration in filter plate 3 Under, filter screen can carry out secondary filter to the gas collected at this temperature, to improve the purity for collecting gas, reduce and collect Other reactions occur in the process.
Wherein, the outlet end of the evaporator 1 is connect with solid-liquid separator, and solid-liquid separator connects with plate and frame type filter-press It connects.
The devices such as solid-liquid separator, plate and frame type filter-press are well known to those skilled in the art in the present embodiment, no longer in detail It states.The main function of solid-liquid separator is that treated that liquid is separated by solid-liquid separation to gas evaporation, and the solid after separation passes through Plate and frame type filter-press carries out press filtration, and press filtration is filled at filter cake shape.
Wherein, one end of the folded sheet 4 is fixed on the inner wall of evaporator 1, and the other end of folded sheet 4 is fixed on partition board On 6, and folded sheet 4 is in continuous Z-shaped.
In the present embodiment, the planform of folded sheet 4 is defined, the main function of folded sheet 4 in a device is pair Gas is drained, it is allowed to be flowed in the predetermined direction, and is flow in getter pipe 5.Therefore folded sheet 4 is in Z-shaped, Z One end of font plate is fixed on the inner wall of evaporator 1, and the other end is fixed on partition board 6, is reduced between partition board 6 and filter plate 3 Space, and the cavity distance between one end of getter pipe 5, filter plate 3 and partition board 6 reduces, then the gas to evaporating Body flow direction guides.
Wherein, the first gas collection device 8, second gas collection device 9, third gas collection device 10 are identical Structure.The concrete structure of first gas collection device 8 is collecting bag or collecting chamber.
Wherein, the filter plate 3 is to bend to interior arcuation, and the radian of bending is 40-60 °.Here the structure of filter plate Can be also arc shape, be in 40-60 ° of radian, and one end of filter plate is on the inner wall of evaporator 1, the other end on partition board 6, this In one end of filter plate be specifically in corresponding with the cavity that isolation board the is enclosed evaporator of filter plate 1 on the inner wall of evaporator On inner wall, meanwhile, filter plate 3 is located at the opposite end of getter pipe 5.
Wherein, the four-way valve 7 is solenoid valve.
Four-way valve 7 is solenoid valve, refers to that can open corresponding flow path as needed, makes the gas being evaporated to corresponding receipts In acquisition means.
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include Within protection scope of the present invention.

Claims (10)

1. a kind of recovery processing technique of organosilicon slag slurry, it is characterised in that:Including following operating procedure,
(1) organosilicon slag slurry is delivered in evaporator using high-pressure pump, preheating temperature uses low-speed mixer to 26-28 DEG C 30-40r/min are stirred, and stir 20-30min, collect tetramethylsilane gas;
(2) 30-40 DEG C are then heated to, with the rotating speed of 20-30r/min, 1h-2h is stirred, collects the trichlorosilane gas of generation Body;
(3) continue to be heated to 75-77 DEG C, with the rotating speed of 30-40r/min, stir 1.5h-2h, collect the tetrachloromethane of generation Gas;
(4) remaining organosilicon slag slurry is passed through buck, is fully reacted, obtain graininess hydrolysate, carry out solid-liquor separation.
2. a kind of recovery processing technique of organosilicon slag slurry according to claim 1, it is characterised in that:The step (1), In step (2), step (3) then the gas of collection is collected by filtering.
3. a kind of recovery processing technique of organosilicon slag slurry according to claim 1 or 2, it is characterised in that:The step (4) after being evaporated gas in, organosilicon slag slurry is transferred in solid-liquid separator, by high-pressure hydraulic pump by buck with 8m/s- The speed of 9m/s is passed into solid-liquid separator, and the copper powder reaction in organosilicon slag slurry generates Kocide SD flocky precipitate, leads to Enter to plate and frame type filter-press, Kocide SD is isolated in press filtration, and gained alkalinity clear liquid is delivered to next treatment process and uses.
4. a kind of recovery processing technique of organosilicon slag slurry according to claim 1, it is characterised in that:The buck is hydrogen Sodium oxide molybdena or potassium hydroxide solution.
5. a kind of organosilicon slag slurry recycling and processing device, it is characterised in that:Including evaporator (1), evaporator (1) is hollow circuit cylinder The lower end periphery of body structure, evaporator (1) is provided with sheathed heater (2), and the inner upper end of evaporator (1) is equipped with filter plate (3), the upper end of filter plate (3) is equipped with partition board (6), and cavity is equipped between partition board (6) and filter plate (3), is equipped with and folds in cavity Plate (4);The upper end of evaporator (1) is additionally provided with getter pipe (5), the input end of getter pipe (5) be in horn-like, getter pipe (5) Input end is located at partition board (6) and is formed by cavity with filter plate (3), and the input end end face of getter pipe (5) is equipped with filter screen, The aperture of filter screen is 0.1-0.3um, and getter pipe (5) is extended to outside evaporator (1) and connect with four-way valve (7), four-way valve (7) three outlets respectively with first gas collection device (8), second gas collection device (9), third gas collection device (10) it connects.
6. a kind of organosilicon slag slurry recycling and processing device according to claim 5, it is characterised in that:The evaporator (1) Outlet end connect with solid-liquid separator, solid-liquid separator is connect with plate and frame type filter-press.
7. a kind of organosilicon slag slurry recycling and processing device according to claim 5, it is characterised in that:The folded sheet (4) One end be fixed on the inner wall of evaporator (1), the other end of folded sheet (4) is fixed on partition board (6), and folded sheet (4) is in Continuous Z-shaped.
8. a kind of organosilicon slag slurry recycling and processing device according to claim 5, it is characterised in that:The first gas is received Acquisition means (8), second gas collection device (9), third gas collection device (10) are identical structure.
9. a kind of organosilicon slag slurry recycling and processing device according to claim 5, it is characterised in that:The filter plate (3) To bend to interior arcuation, the radian of bending is 40-60 °.
10. a kind of organosilicon slag slurry recycling and processing device according to claim 5, it is characterised in that:The four-way valve (7) For solenoid valve.
CN201810448036.4A 2018-05-11 2018-05-11 A kind of recovery processing technique and its processing unit of organosilicon slag slurry Pending CN108607267A (en)

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CN201810448036.4A CN108607267A (en) 2018-05-11 2018-05-11 A kind of recovery processing technique and its processing unit of organosilicon slag slurry

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Publication number Priority date Publication date Assignee Title
GB2468741A (en) * 2009-02-27 2010-09-22 Nano Porous Solutions Ltd Separation device with exhaust silencer
CN102390860A (en) * 2011-08-04 2012-03-28 山东东岳有机硅材料有限公司 Environmentally-friendly treatment method and device for organosilicon slurry
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Application publication date: 20181002