CN109897058A - A kind of organic silicon slurry slag processing system and treatment process - Google Patents
A kind of organic silicon slurry slag processing system and treatment process Download PDFInfo
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- CN109897058A CN109897058A CN201910153411.7A CN201910153411A CN109897058A CN 109897058 A CN109897058 A CN 109897058A CN 201910153411 A CN201910153411 A CN 201910153411A CN 109897058 A CN109897058 A CN 109897058A
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Abstract
The invention belongs to Waste Disposal Technology fields, disclose a kind of organic silicon slurry slag processing system and treatment process, the entrance of azeotropic vaporization kettle device is connect with the blending tank in mixing organic silicon slurry slag source and azeotropic solvent, by the silane substance in screenings together with solvent azeotropic vaporization, obtained evaporation product, which enters, steams product rectifying column, and tower reactor obtains high boiling organosilicon liquid monomer product, which send to high boiling cracker, active principle is recycled, the azeotropic solvent that tower top obtains is for reusing；After raffinate in azeotropic vaporization kettle device is filtered and is dried, device is inactivated into useless powder, extracts and recycles the components such as valuable copper, silicon.The present invention is evaporated the operation such as rectifying to the organic silicon slurry slag for being difficult to handle, valuable monomer can be recycled, produce higher boiling methylchlorosilane, higher boiling methylchlorosilane useful in screenings is set to recycle, realize the minimizing processing of organic silicon slurry slag, production cost is greatly reduced, there is preferable economic benefit.
Description
Technical field
The invention belongs to Waste Disposal Technology fields, in particular to a kind of processing system of organic silicon slurry slag
And treatment process.
Background technique
Organosilicon waste pulp slag refers to a kind of liquid-solid mixture of the mobility generated in methyl chlorosilane monomer synthesis process,
It is more than mainly that 70 DEG C of high-boiling components and a small amount of fine silicon powder, copper powder form by boiling point.Organic silicon slurry slag belongs to danger wastes,
Its form in high-boiling components it is inflammable and explosive, high volatility can burn or react shape with air if exposure is in air
At strong acid mist or strong acid liquid.In addition, the silicon powder in screenings also belongs to combustible material, if copper powder is easy to provide water without recycling
Source pollutes, if this kind of organosilicon waste pulp slag direct emission can cause environment seriously to pollute, it is therefore necessary to carry out without public affairs
Evilization processing.
Currently, main waste pulp slag environmentally friendlyization processing method is Hydrolyze method and cracking process.Being handled using Hydrolyze method is had
Machine silicon screenings, mainly to organic silicon slurry slag hydrolyze pre-treatment or use different hydrolysis mediums, obtain it is inert, do not stick,
Segregative hydrolysis composition granule and the hydrating solution for meeting discharge standard；Organic silicon slurry slag, mainly handle are handled using cracking process
Single silane is made in high-boiling components cracking in screenings, to recycle active principle, realizes recycling for screenings.In addition, domestic organic
Silicon industry also carries out harmless treatment to organic silicon slurry slag using a kind of new technology incineration method, i.e., with a certain amount of excess air and
Fuel carries out oxidizing fire with organic screenings to be processed in incinerator and reacts, and the substance in screenings is at 800 DEG C~1200 DEG C
At a high temperature of oxidation, pyrolysis and be destroyed, thus realize processing organic silicon slurry slag purpose.
CN106220666A discloses " a kind of processing system and processing method of organic silicon slurry slag ", including organic silicon slurry slag
Source, heating and evaporating unit and condensate recycling device.Wherein, the entrance of heating and evaporating unit is connect with organic silicon slurry slag source, is added
Heat evaporating device provides environment under low pressure, and heats to organic silicon slurry slag；The entrance and heating evaporation of condensate recycling device fill
The upper end outlet connection set carries out condensing recovery to the gaseous phase materials that organic silicon slurry slag heating evaporation comes out.
CN101659672A discloses " a kind of method for cracking treatment of organic silicon waste residue slurry ", and organic silicon waste residue slurry is consolidated and is contained
The liquid-solid mixture that amount is 20% is added the high-boiling components of phase homogenous quantities, is made into cracking stock liquid；Catalyst is tri-n-butylamine, cracking
Optimal reaction temperature is 120 DEG C~130 DEG C；It is passed through HCl gas, hydrogen chloride charging rate and mixed liquor are most preferably than for 1:1.10.
Pyrolysis product obtains single silane by rectification and purification, wherein unreacted raw material and solid residue are using at method for hydrolysis
Reason.
CN202109493U discloses " the screenings Special incineration equipment generated in a kind of organic silicon production process ", including combustion
Device, dust-extraction unit, acid dip pickle and alkaline cleaner are burnt, the burner outlet is connected with the entrance of the dust-extraction unit
It connects, the outlet of the dust-extraction unit is connected with the entrance of the acid dip pickle, the outlet of the acid dip pickle and the alkali cleaning
The entrance of device is connected.
In the several method being generally noted above, the shortcomings that Hydrolyze method, is that hydrolysis rate relatively slowly and hydrolysis is insufficient, obtains
To hydrolysate be difficult to carry out subsequent separation process, domestic technology for hydrolyzing generally falls behind, and this method has air and water environment
Serious pollution problem；The shortcomings that cracking process is that temperature asks higher, is easy carbon distribution, and catalyst is expensive, higher cost；It burns
The shortcomings that burning method is that temperature requirement is too high, and pickling alkali cleaning is needed to generate secondary pollution and waste liquid, and the silane substance in screenings
It is destroyed, results in waste of resources.Therefore, organosilicon waste pulp slag can need to be reduced using a kind of environmentally friendly method
Change processing, and valuable silane substance and copper in screenings can be recycled, the components such as silicon.
Summary of the invention
The technical problems such as waste for the secondary pollution occurred in existing organic silicon slurry slag treatment process and efficient resource,
The invention discloses a kind of effective organic silicon slurry slag processing system and treatment process, can be reduced to organosilicon waste pulp slag
Change, harmless treatment, and the components such as the silane substance in screenings and valuable copper, silicon can be recycled.
In order to solve the above-mentioned technical problem, the present invention is achieved by technical solution below:
A kind of organic silicon slurry slag processing system, including screenings slot, azeotropic solvent tank, blending tank, azeotropic vaporization kettle, steam production
Product rectifying column, high boiling cracker, residual filter, solid drying tower, useless powder inactivate device；
The screenings slot and the azeotropic solvent tank are connected with the blending tank, and the blending tank is for storing and stirring
Mix organic silicon slurry slag raw material and azeotropic solvent；
The outlet of the blending tank is connect with the entrance of the azeotropic vaporization kettle, and the material outlet of the azeotropic vaporization kettle is logical
The first pumping unit is crossed to be connected with the feed entrance for steaming product rectifying column, the top export for steaming product rectifying column with
The azeotropic solvent tank is connected, and partial solvent is back to the top of the distillation column by the second pumping unit in the azeotropic solvent tank, institute
It states and steams the bottom end outlet of product rectifying column and be connected by third pumping unit with the high boiling cracker；
The raffinate outlet of the azeotropic vaporization kettle is connected with the entrance of the residual filter, and the residual filter goes out
Mouth is connected with the entrance of the solid drying tower, and the outlet of the solid drying tower is connected with the useless powder inactivation device.
Further, the azeotropic solvent is monochloro methane, methylene chloride, chloroform or tetrachloroethanes.
Further, the azeotropic vaporization kettle uses batch reactor or continuous reaction kettle, is internally provided with stirring
Paddle, outside are provided with heating device.
Further, the azeotropic vaporization kettle uses electric heating, hot water heating, conduction oil circulating-heating, Far-infrared Heating
Or inside/outside coil pipe heating.
Further, the azeotropic vaporization kettle is provided with temperature instruction control system, and temperature instruction control system is for surveying
Determine real time temperature in kettle and is compared with set temperature；When real time temperature reaches set temperature in kettle, the temperature instruction
Control system controls the azeotropic vaporization kettle and stops heating.
Further, the azeotropic vaporization kettle is provided with liquid level instruction control system, and the liquid level instruction control system is used
It is compared in azeotropic mixture liquid level in measurement kettle and with setting value；When azeotropic mixture liquid level is lower than setting value in kettle, the liquid level
Indicate that control system controls the azeotropic vaporization kettle and stops evaporation.
Further, for the product rectifying column that steams using plate column, plate column column plate uses sieve plate column plate or valve tower
Plate；The product rectifying tower that steams is top-loaded with condenser, and tower bottom is equipped with reboiler.
Further, the solid drying tower is furnished with the dedicated air blower of drying equipment.
Further, the solid drying tower is using constant pressure and dry, nitrogen displacement drying or vacuum drying.
A kind for the treatment of process of the organic silicon slurry slag processing system, this method follow the steps below:
(1) it after organic silicon slurry slag and azeotropic solvent mix, is heated in the azeotropic vaporization kettle, makes the silicon in screenings
Alkane substance and solvent azeotropic vaporization together, the evaporation product that the azeotropic vaporization kettle obtains enter described in steam product rectifying column；
(2) the product rectifying column that steams is to evaporation product progress rectifying separation, and tower top obtains low-boiling solvent, through cold
It returns to the azeotropic solvent tank after solidifying to be reused, tower bottom obtains the high boiling high boiling monomer of organosilicon liquid phase, the monomer
Into the high boiling cracker；
(3) the high boiling cracker carries out high boiling cracking to the high boiling monomer of organosilicon liquid phase, recycles active principle, production
Higher boiling methylchlorosilane；
(4) after azeotropic vaporization kettle 4 stops evaporation, raffinate in kettle is successively done by the residual filter and the solid
After dry tower is filtered, dries, solid powder enters the useless powder and inactivates device；
(5) the useless powder inactivation device is recycled the organosilicon powder that gives up.
The beneficial effects of the present invention are:
(1) organic silicon slurry slag processing processing system and treatment process provided by the invention, waste pulp slag and solvent are total to
After boiling evaporation, rectification and purification is carried out, the processes such as high boiling cracking produce higher boiling methylchlorosilane, make higher boiling useful in screenings
Methylchlorosilane is recycled, while by being filtered drying to raffinate, recycling the groups such as valuable silicon, copper in screenings
Point, it really realizes the minimizing processing of organic silicon slurry slag, substantially increases the utilization efficiency of useful material in screenings.
(2) organic silicon slurry slag processing processing system and treatment process provided by the invention, avoid screenings direct hydrolysis band
The waste hydrochloric acid come, the environmental problem of the secondary pollutions such as waste water, with cracking process compared with incineration method, operating condition milder is not necessarily to
High mild catalyst.
(3) organic silicon slurry slag processing processing system and treatment process provided by the invention, can directly utilize organosilicon work
The existing apparatus of factory, reduces costs, and saves investment, and azeotropic solvent can reuse after rectifying separation condensation, accord with
Close energy-saving and environmental protection, the requirement of extra earning.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of organic silicon slurry slag processing system provided by the present invention.
In figure: 1. slurry slots；2. azeotropic solvent tank；3. blending tank；4. azeotropic vaporization kettle；5. residual filter；6. solid
Drying tower；7. air blower；8. useless powder inactivates device；9. the first pumping unit；10. the second pumping unit；11. third pumping unit；12. steaming
Product rectifying column out；13. high boiling cracker.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail, and following embodiment can make this profession
The present invention, but do not limit the invention in any way is more completely understood in technical staff.
As shown in Figure 1, the present embodiment makes public for the first time a kind of organosilicon slurry for collecting the processes one such as evaporation, rectifying, cracking
Slag disposal system, mainly include screenings slot 1, azeotropic solvent tank 2, blending tank 3, azeotropic vaporization kettle 4, steam product rectifying column 12,
High boiling cracker 13, residual filter 5, solid drying tower 6, useless powder inactivate device 8.
The screenings slot 1 and azeotropic solvent tank 2 of organosilicon are connected with the two entrances of blending tank 3 respectively, and blending tank 3 is used for
Organic silicon slurry slag raw material and azeotropic solvent are stored, is also used to stir organic silicon slurry slag, is sufficiently mixed it with azeotropic solvent.
Azeotropic solvent is monochloro methane, methylene chloride, chloroform, tetrachloroethanes etc..
The outlet of blending tank 3 is connect with the entrance of azeotropic evaporating kettle 4, after organic silicon slurry slag and azeotropic solvent mixing, altogether
It is heated in boiling evaporating kettle 4, makes silane substance in screenings and solvent azeotropic vaporization together.Azeotropic vaporization kettle 4 uses interval
Formula reaction kettle or continuous reaction kettle are internally provided with agitating paddle, and outside is provided with heating device, and organic silicon slurry slag and azeotropic are molten
Agent is able to carry out under the action of heating and stirring and comes into full contact with dissolution, keeps slurry temperature more uniform, improves evaporation effect
Rate.Electric heating, hot water heating, conduction oil circulating-heating, Far-infrared Heating, inside/outside can be used in the heating method of azeotropic vaporization kettle 4
Coil pipe heating etc..
Azeotropic vaporization kettle 4 is provided with temperature instruction control system and is added when real time temperature is lower than set temperature in kettle
Heat；When real time temperature is equal to or higher than set temperature in kettle, stop heating.Azeotropic vaporization kettle 4 is provided with liquid level instruction control
System stops evaporation when azeotropic mixture liquid level is lower than setting value in kettle.
The material outlet of azeotropic vaporization kettle 4 is connected by the first pumping unit 9 with the feed entrance for steaming product rectifying column 12,
Product rectifying column 12 is steamed using plate column, plate column column plate uses sieve plate or valve plate；Tower top is equipped with condenser, tower bottom dress
There is reboiler.The top export for steaming product rectifying column 12 is connected with azeotropic solvent tank 2, and the solvent of tower top output returns after condensing
Azeotropic solvent tank 2 is returned, azeotropic solvent is enable to recycle.Partial solvent in azeotropic solvent tank 2 passes through the second pumping unit 10
It is back to the top of the distillation column.The bottom end outlet for steaming product rectifying column 12 passes through third pumping unit 11 and high boiling 13 phase of cracker
Even, the organic silicon monomer of tower bottom output is made to enter high boiling cracker 13.High boiling cracker 13 is to steaming product rectifying column 12
The high boiling organosilicon monomer of production carries out high boiling cracking, recycles active principle, produces higher boiling methylchlorosilane.
The raffinate outlet of azeotropic vaporization kettle 4 is connected with the entrance of residual filter 5, the outlet of residual filter 5 and solid
The entrance of drying tower 6 is connected.Residual filter 5 carries out raffinate filtering to the raffinate of azeotropic vaporization kettle 4.Solid drying tower 6 is to residual
The filtered solid powder of liquid is dried, and is furnished with the dedicated air blower 7 of drying equipment；Solid drying mode uses constant pressure and dry,
Nitrogen displacement drying, or vacuum drying.
The outlet of solid drying tower 6 is connected with the entrance of useless powder inactivation device 8.Useless powder inactivation device 8 gives up powder to organosilicon
It is recycled, extracts the components such as valuable copper, silicon.
Based on the treatment process of above-mentioned organic silicon slurry slag processing system, carry out in accordance with the following steps:
(1) it after organic silicon slurry slag and azeotropic solvent mix, is heated in azeotropic vaporization kettle 4, makes the silane in screenings
Azeotropic vaporization, the evaporation product entrance that azeotropic vaporization kettle 4 obtains steam product rectifying column 12 together for substance and solvent；
(2) it steams product rectifying column 12 and rectifying separation is carried out to evaporation product, tower top obtains low-boiling solvent, through condensing
It returns to azeotropic solvent tank 2 afterwards to be reused, tower bottom obtains the high boiling high boiling monomer of organosilicon liquid phase, which enters height
Boil cracker 13；
(3) high boiling cracker 13 carries out high boiling cracking to the high boiling monomer of organosilicon liquid phase, recycles active principle, and production is high
Boiling point methylchlorosilane；
(4) after azeotropic vaporization kettle 4 stops evaporation, raffinate in kettle is successively passed through into residual filter 5 and solid drying tower 6
After being filtered, drying, solid powder enters useless powder and inactivates device 8；
(5) the powder inactivation device 8 that gives up is recycled the organosilicon powder that gives up, and extracts the components such as valuable copper, silicon.
Although the preferred embodiment of the present invention is described above in conjunction with attached drawing, the invention is not limited to upper
The specific embodiment stated, the above mentioned embodiment is only schematical, be not it is restrictive, this field it is common
Technical staff under the inspiration of the present invention, without breaking away from the scope protected by the purposes and claims of the present invention, may be used also
By make it is many in the form of specific transformation, within these are all belonged to the scope of protection of the present invention.
Claims (10)
1. a kind of organic silicon slurry slag processing system, which is characterized in that including screenings slot, azeotropic solvent tank, blending tank, azeotropic vaporization
Kettle steams product rectifying column, high boiling cracker, residual filter, solid drying tower, useless powder inactivation device；
The screenings slot and the azeotropic solvent tank are connected with the blending tank, and the blending tank is for storing and having stirred
Machine silicon screenings raw material and azeotropic solvent；
The outlet of the blending tank is connect with the entrance of the azeotropic vaporization kettle, and the material outlet of the azeotropic vaporization kettle passes through the
One pumping unit is connected with the feed entrance for steaming product rectifying column, the top export for steaming product rectifying column with it is described
Azeotropic solvent tank is connected, and partial solvent is back to the top of the distillation column, the steaming by the second pumping unit in the azeotropic solvent tank
The bottom end outlet of product rectifying column is connected by third pumping unit with the high boiling cracker out；
The azeotropic vaporization kettle raffinate outlet is connected with the entrance of the residual filter, the outlet of the residual filter and
The entrance of the solid drying tower is connected, and the outlet of the solid drying tower is connected with the useless powder inactivation device.
2. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the azeotropic solvent is a chlorine
Methane, methylene chloride, chloroform or tetrachloroethanes.
3. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the azeotropic vaporization kettle uses
Batch reactor or continuous reaction kettle, are internally provided with agitating paddle, and outside is provided with heating device.
4. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the azeotropic vaporization kettle uses
Electric heating, hot water heating, conduction oil circulating-heating, Far-infrared Heating or the heating of inside/outside coil pipe.
5. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the azeotropic vaporization kettle setting
There is temperature to indicate control system, temperature instruction control system is for measuring real time temperature in kettle and being compared with set temperature；
When real time temperature reaches set temperature in kettle, the temperature instruction control system controls the azeotropic vaporization kettle and stops heating.
6. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the azeotropic vaporization kettle setting
There is liquid level to indicate control system, the liquid level instruction control system is for measuring azeotropic mixture liquid level in kettle and being compared with setting value
Compared with；When azeotropic mixture liquid level is lower than setting value in kettle, the liquid level instruction control system controls the azeotropic vaporization kettle and stops steaming
Hair.
7. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that described to steam product rectifying column
Using plate column, plate column column plate uses sieve plate column plate or valve plate；The product rectifying tower that steams is top-loaded with condenser,
Tower bottom is equipped with reboiler.
8. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the solid drying tower is furnished with
The dedicated air blower of drying equipment.
9. a kind of organic silicon slurry slag processing system according to claim 1, which is characterized in that the solid drying tower uses
Constant pressure and dry, nitrogen displacement drying or vacuum drying.
10. a kind for the treatment of process based on the organic silicon slurry slag processing system as described in any one of claim 1-9, feature exist
In this method follows the steps below:
(1) it after organic silicon slurry slag and azeotropic solvent mix, is heated in the azeotropic vaporization kettle, makes the silane object in screenings
Matter and solvent azeotropic vaporization together, the evaporation product that the azeotropic vaporization kettle obtains enter described in steam product rectifying column；
(2) the product rectifying column that steams is to evaporation product progress rectifying separation, and tower top obtains low-boiling solvent, after condensing
It returns to the azeotropic solvent tank to be reused, tower bottom obtains the high boiling high boiling monomer of organosilicon liquid phase, which enters
The high boiling cracker；
(3) the high boiling cracker carries out high boiling cracking to the high boiling monomer of organosilicon liquid phase, recycles active principle, produces high boiling
Point methylchlorosilane；
(4) after azeotropic vaporization kettle 4 stops evaporation, raffinate in kettle is successively passed through into the residual filter and the solid drying tower
After being filtered, drying, solid powder enters the useless powder and inactivates device；
(5) the useless powder inactivation device is recycled the organosilicon powder that gives up.
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| CN110433507A (en) * | 2019-08-08 | 2019-11-12 | 江西蓝星星火有机硅有限公司 | A method of according to solid content automatic-discharging silane screenings |
| CN114262792A (en) * | 2021-12-01 | 2022-04-01 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry residue hydrolysis treatment process and resource recycling method |
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| CN115106045A (en) * | 2022-07-26 | 2022-09-27 | 乐山协鑫新能源科技有限公司 | High-boiling treatment system for slag slurry |
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| CN115106045A (en) * | 2022-07-26 | 2022-09-27 | 乐山协鑫新能源科技有限公司 | High-boiling treatment system for slag slurry |
| CN115106045B (en) * | 2022-07-26 | 2024-03-29 | 乐山协鑫新能源科技有限公司 | High-boiling treatment system for slurry |
| WO2024035253A1 (en) * | 2022-08-11 | 2024-02-15 | Especialidades Químicas Globales De México, S.A.P.I. De C.V. | Process for purifying and deodorising silicone used for the washing of cosmetics production lines |
| CN115475825A (en) * | 2022-09-29 | 2022-12-16 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry slag treatment process |
| CN115475825B (en) * | 2022-09-29 | 2023-06-27 | 鲁西化工集团股份有限公司硅化工分公司 | Organosilicon slurry residue treatment process |
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Application publication date: 20190618 |