CN108409780A - A kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method and device of circulation - Google Patents
A kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method and device of circulation Download PDFInfo
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- CN108409780A CN108409780A CN201810450308.4A CN201810450308A CN108409780A CN 108409780 A CN108409780 A CN 108409780A CN 201810450308 A CN201810450308 A CN 201810450308A CN 108409780 A CN108409780 A CN 108409780A
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- 239000002904 solvent Substances 0.000 title claims abstract description 57
- 230000004087 circulation Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000003776 cleavage reaction Methods 0.000 title claims abstract description 18
- 230000007017 scission Effects 0.000 title claims abstract description 18
- 238000005336 cracking Methods 0.000 claims abstract description 112
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 238000009834 vaporization Methods 0.000 claims abstract description 3
- 230000008016 vaporization Effects 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 40
- 239000000413 hydrolysate Substances 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 241000628997 Flos Species 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 5
- 230000008707 rearrangement Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004523 catalytic cracking Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- -1 Siloxanes Chemical class 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003416 augmentation Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003818 cinder Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009089 cytolysis Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000007792 gaseous phase Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 230000001839 systemic circulation Effects 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000012962 cracking technique Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- LLPOLZWFYMWNKH-CMKMFDCUSA-N hydrocodone Chemical compound C([C@H]1[C@H](N(CC[C@@]112)C)C3)CC(=O)[C@@H]1OC1=C2C3=CC=C1OC LLPOLZWFYMWNKH-CMKMFDCUSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The present invention relates to organosilicon hydrolyzation object cleavage methods and device that a kind of solvent naphtha heat drives circulation,The double helix channel of class spiral-plate heat exchanger form is coaxially disposed in the middle part of cracker,Helical duct upper and lower ends blow-by one of in double helix channel,As cracking channel,Another helical duct upper and lower ends sealing,Form heat exchanging medium passage,Solvent naphtha is distributed in the annular space between the cylinder and cracker of cracking channel and double helix channel composition,Organosilicon hydrolyzation object and the mixture of KOH solution are sent into cracking channel,The heat transferring medium of heat exchanger channels provides heat for cracking channel,Organosilicon hydrolyzation object mixes in cracking channel with solvent naphtha,Side border ring vaporization,Bubble, which rises, drives the liquid in cracking channel to rise to cracking channel roof,After gas-liquid separation,Solvent naphtha,Unreacted organosilicon hydrolyzation object drops to cracker bottom with KOH solution by annular space,Form Natural Circulation.Present invention device without mixing, heat transfer, mass-transfer efficiency are high, not will produce hot-spot phenomenon, and the device production cycle increases, and alkali consumption is reduced, and improves ring body yield and D4, DMC quality, it is stable operation, safe and reliable.
Description
Technical field
The present invention relates to chemical production technical fields, and in particular to the organosilicon hydrolyzation object that a kind of solvent naphtha heat drives circulation is split
Solve method and device.
Background technology
In silicone industry, 85% or more organosilicon product and product are by silicone intermediate (such as prestox ring four
Siloxanes D4, dimethicone mixture D MC) production, therefore, dimethyldichlorosilane (abbreviation diformazan) hydrolysate
Cracking is reset particularly important.Cracking process is exactly that from the external world, heat absorption carries out cracking weight to diformazan hydrolysate under the conditions of basic catalyst
Row's reaction contains 60% or so D to be made4, 10% or so D3With 20% or so D5Lysate, referred to as dimethicone is mixed
Object (DMC) is closed, the D that purity is more than 99% (mass fraction) can be made by further rectifying4Product.Contain during cracking reaction
The siloxanes of trifunctional or Si-H become silanol sylvite, stay in the bottom of cracking still.
In organic silicon monomer cracking production, two kinds of techniques, and two kinds are generally cracked using dry method cracking and solvent oil process
Process route has all realized industrialized production.Currently, domestic cracker mostly uses dry method cracking technology, i.e. hydrolysate vapour
Change, crack, being evaporated and ring body washing semicontinuous cracking technology route.Technics comparing is ripe, the D of major product4, DMC ratios
It can suitably be adjusted according to market situation, and with " D in DMC4+D5" based on.But the technique is there are ring body yield is low, product
The problems such as of poor quality, the parking deslagging period is short, and alkali consumption is big, key equipment uneven heating, amplification difficulty.
Alkali can not only be such that Si-O-Si keys are broken at high temperature, while also be broken a certain number of Si-C keys, thus straight
The polymer of cross-linked structure can be generated in the cracking process of chain polysiloxanes.It, can be anti-by alkaline lysis to avoid the fracture of Si-C keys
It should be carried out in high boiling atent solvent.
Foreign countries just have the patent report that solvent method cracking diformazan hydrolysate prepares cyclosiloxane from the beginning of the eighties.By solvent naphtha
It is added in cracking still as heat carrier, keeps cracking reaction heat transfer uniform, eliminate hot-spot phenomenon, control disproportionated reaction
Generation, improve ring body yield.
Key equipment in solvent method continuous cracking technique is cracking still, and relatively common at present is to have chuck, inside outside
Stirring-type cracking still with heating coil.Chinese invention patent application CN201210221210.4 discloses a kind of organosilicon cracking
Reactor stirs leaves structure shortens the distance of paddle and bottom, carries although bottom stirring leaf shape is consistent with arc kettle
High mixed effect, however the presence of agitating device, equipment leakproofness cannot ensure that safety is not high.For in negative pressure item
The cracking reaction carried out under part is easy sucking air and generates explosive atmosphere, and there are hidden danger for safety in production.
Chinese utility model patent 201620965364.8 discloses a kind of organic silicon cracking device, and disk is arranged in cracking still body
Heat exchange of heat pipe and double-U-shaped pipe heater, although improving heating surface (area) (HS and the efficiency of heating surface, near coil pipe and U-tube device
Temperature of charge is high, and other positions temperature is low, and heating is uneven, will produce side reaction, and coil pipe and U-tube bending part are easily heavy
Contamination dirt.
For above-mentioned cracking still due to the presence of chuck, external pressure suffered by shell increases to 1MPa (pressure of heating steam), above-mentioned to split
Solution still shell body thickness necessarily increases, and increases material consumption.Design when also need to consider take over, manhole and chuck are mutually kept away
Allow, weld strength and safety, weld seam are suitable for factors such as arrangements, keep cracking still complicated, improve cost；Easy to produce stirring
Dead angle, the fouling on heating surface, makes heat transfer efficiency decline, and reaction efficiency is lower, and cracking still bottom can accumulate a large amount of silanol potassium
Salt needs scarfing cinder of often stopping, is easy to happen explosion, seriously affects the production of cyclosiloxane.
Invention content
For current organosilicon industry crack reset kettle the state of the art, there are the drawbacks of and deficiency, of the invention first
A purpose is to provide a kind of organosilicon hydrolyzation object cleavage method of solvent naphtha heat drive circulation, is passed in mass transfer with solving traditional cracking still
Heat is sufficiently mixed, the deficiency in terms of the production cycle, while improving safety.
A kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method of circulation, and class spiral is coaxially disposed in the middle part of cracker
The double helix channel of sheet heat exchanger form, helical duct upper and lower ends blow-by one of in double helix channel, as splitting
Channel is solved, another helical duct upper and lower ends sealing forms heat exchanging medium passage, solvent naphtha is in cracking channel and double helix channel
It is distributed in annular space between the cylinder and cracker of composition, the mixture of organosilicon hydrolyzation object and KOH solution is sent into cracking channel
In, the heat transferring medium of heat exchanger channels provides heat for cracking channel, and organosilicon hydrolyzation object mixes in cracking channel with solvent naphtha,
Side border ring vaporization, bubble, which rises, drives the liquid in cracking channel to rise to cracking channel roof, after gas-liquid separation, solvent
Oily, unreacted organosilicon hydrolyzation object and KOH solution drop to cracker bottom by annular space, form Natural Circulation.
Compared with prior art, double helix channel can augmentation of heat transfer, provide institute's calorific requirement to react in time, and can promote
Mass transfer, feature are that rate of heat transfer is fast, and reactant system temperature equalization, reactant reaction is abundant, reduces the generation of by-product.
In order to liquid enter cracking channel it is more uniform, it is preferred that cracker bottom be arranged liquid distribution trough, pass through
Organosilicon hydrolyzation object and the mixture of KOH solution are sent into cracking channel by liquid distribution trough.
Preferably：After reaction, gas-liquid is in cracking channel roof separation, by cracking after the gas removal solvent naphtha isolated
Device gas outlet is discharged.
Preferably：Inverted cone segment and floss hole is arranged in cracker bottom, reacts the cracking slag of generation in inverted cone segment through weight
After power sedimentation, discharged from floss hole.The flowing of inverted cone segment overhead-liquid is gentle, and lower liquid is essentially stationary state, reaction
The cracking slag of generation is assembled through gravitational settling in centrum in conical section, is discharged from floss hole, it is continuous that long period may be implemented
Production, and eliminate security risk.
Second object of the present invention is to provide a kind of organosilicon hydrolyzation object cracker of solvent naphtha heat drive circulation, cracking
Device includes feed inlet, gas outlet, heat transferring medium entrance, heat transferring medium outlet, solvent oil-in, floss hole, feed inlet setting
In cracker lower part side, gas outlet setting exports in cracker top center, heat transferring medium entrance, heat transferring medium, is molten
The setting of agent oil-in is arranged in cracker top, floss hole in cracker bottom centre；Coaxial arrangement in the middle part of cracker
The double helix channel of class spiral-plate heat exchanger form, helical duct upper and lower ends blow-by one of in double helix channel,
As cracking channel, another helical duct upper and lower ends sealing forms heat exchanging medium passage, solvent naphtha is in cracking channel and double spiral shells
It is distributed in annular space between the cylinder and cracker of rotation channel composition, liquid distribution trough, liquid distribution trough is arranged in feed inlet top
Organosilicon hydrolyzation object and the mixture of KOH solution are sent into cracking channel.
Compared with prior art, the configuration of the present invention is simple, without clamping device, do not have agitating device, due to class spiral plate
Structure has automatic cleaning action, and solvent naphtha is in the annular space between the cylinder and cracker of cracking channel and double helix channel composition
The problem of circulating, substantially reducing fouling, double helix channel are both heat exchanger channels and mass transfer channel and reaction zone, are passed
Hot rate is fast, and reactant system temperature equalization, reactant mass transfer is abundant, reduces the generation of by-product, increases the receipts of ring body
Rate.
The spacing in double helix channel is adjustable, to ensure heat transfer effect and mass transfer effect.The spacing in channel is cracked according to device
Production capacity and heat exchange area design；The spacing of heat exchanger channels can be designed according to the internal circulating load of heat transferring medium, by promoting heat transferring medium
Flowing velocity, improve heat transfer coefficient, augmentation of heat transfer effect.
The annular space spacing that heat drives inside circulation type cracking still body can be also designed according to internal circulating load.
Preferably：Cracker includes top seal head section, middle part cylindrical section and bottom inverted cone segment, and double helix channel is in
Portion's cylindrical section setting, and it is coaxial with cylindrical section；Preferably, demister is set between middle part cylindrical section and top seal head section, with
The solvent naphtha and unreacted hydrolysate and KOH solution carried secretly in separation gas.
Preferably：Liquid distribution trough is made of coil pipe, and fluid injector is arranged on coil pipe, and nozzle vertically upward, or is arranged
It is inserted upwardly into the standpipe in cracking channel, corresponding cracking channel realizes that liquid is uniformly distributed.
Preferably：Floss hole is arranged in lower inverted cone segment bottom.
Third object of the present invention is to provide a kind of solvent naphtha heat drive circulation organosilicon hydrolyzation object continuous cracking system,
Including sequentially connected hydrolysate heater, as described in claim 5-8 is any cracker, cleavage column, reset condenser, water
Wash kettle, D3Tower, hydrolysate tank, product tower, D4Storage tank, cleavage column tower reactor side line connect cracker, and condensation is reset in tower top connection
Device, D3Column overhead connects D3Condenser connects hydrolysate tank, D through pump3Tower connects product tower, and it is cold that product column overhead connects product tower
Condenser, and connect finished product D4Storage tank, product tower side line connect DMC storage tanks, and product tower tower reactor connects hydrolysate tank through pump,.
Compared with prior art, cracker of the invention can discharge cracking slag at work, and need not stop scarfing cinder, disappear
In addition to security risk, it ensure that being carried out continuously for cracking reaction, improve lysis efficiency.
Fourth object of the present invention is to provide a kind of side of the organosilicon hydrolyzation object continuous cracking of solvent naphtha heat drive circulation
Method, step are：Organosilicon hydrolyzation object through the preheating of hydrolysate heater is mixed into proportion with KOH solution such as claim 4-
7 any crackers, carry out catalytic cracking reaction under the action of heat carrier solvent naphtha, and the gas after cyclisation is reset is direct
Into cleavage column, the wire body in tower reactor returns cracking still, and tower top ring body is sent by resetting condenser condensation in purification system
Washing kettle enters D after desalted water purification and washing3Tower, overhead vapours is through D3It is produced by certain reflux ratio after condenser condensation, warp
It is pumped into hydrolysate tank, tower reactor liquid is delivered to product tower, and overhead vapours presses certain reflux ratio after the condensation of product tower condenser
Finished product D is sent into extraction4Storage tank, lateral line discharging is DMC in tower, is sent into DMC storage tanks, and tower reactor epipodium returns after delivery pump pressurizes
Hydrolysate tank；Cracking slag in cracker is discharged through floss hole, is sent to out-of-bounds buried.
Advantages of the present invention：
(1) using double helix channel heat transfer distances are short, the temperature difference is small, the coefficient of heat transfer is high, heat exchange area is big, volumetric specific power
Greatly, the good advantage of flow stability, under isothermal condition, hydrolysate, solvent naphtha mixing mass transport process are quick, and heat transfer is uniform
Efficiently, reaction is abundant, and by-product is few；Product after cracking is gas phase, therefore the fluid in channel boils in flowing, and fluid is violent
Ground turbulence makes to come into full contact with and mix between hydrolysate and catalyst, is conducive to the progress of reaction.
(2) convection current and systemic circulation of liquid are realized in equipment in a manner of hot drive.On the one hand, solvent is recycled in cracking channel
Under the washing away of oil, heat exchange surface is not likely to produce precipitation and dirt, has the effect of self-cleaning, can guarantee continuous and steady operation.It is another
Aspect, reaction product are gas phase, and bubble, which rises, drives solvent naphtha to circulate, and it is anti-to be conducive to cracking for augmentation of heat transfer, mass transfer effect
The abundant progress answered improves product ring body yield.
(3) since reaction is to carry out under vacuum, the requirement to leakproofness is especially high, if leakproofness is not achieved,
Air enters in cracking still, is mixed with siloxanes steam, can form explosive atmosphere, generates dangerous.Without being installed blender
It can be to avoid since the problem of poor sealing, the safety is improved caused by installation blender.
(4) quantity-produced process is basically reached, cracking system can be formed highly concentrated without being evaporated kettle in cracker
The cracking slag of degree, without parking, intermittent discharge.
(5) solvent naphtha cycle uses hydrocone type structure, there is rate of heat transfer height, stable operation, scaling property can wait well excellent
Point.Boiling can avoid slug flow occur in annular space, and operation is stablized compared with blank pipe, while rise and fall stream stock road, it is therefore prevented that steam
Vapour rising is obstructed.The power density of liquid is larger in circular passage, can also obtain optimum value by adjusting annular space width, from
And greatly improve heat transfer coefficient.
Present invention device without mixing, heat transfer, mass-transfer efficiency are high, not will produce hot-spot phenomenon, and the device production cycle increases
Long, alkali consumption is reduced, and improves ring body yield and D4, DMC quality, it is stable operation, safe and reliable.
Description of the drawings
Fig. 1 is that the heat of the present invention drives the structural schematic diagram of circulation type cracking still.
Wherein：101 cracking autoclave bodies, 102 demisters, 103 spiral heat exchangers, 104 liquid distribution troughs, 105 annular spaces,
106 feed inlets, 107 gas outlets, 108 heat transferring medium entrances, the outlet of 109 heat transferring mediums, 110 solvent oil-ins, 111 floss holes.
Fig. 2 is convection current and the systemic circulation model schematic that liquid is realized in a manner of hot drive of the present invention
Fig. 3 is the structural schematic diagram of the present invention
Wherein：1 hydrolysate, 2 hydrolysate heaters, 3 heat drive circulation type cracking still, and 4KOH NaOH solution tank NaOHs, 5 cleavage columns, 6 reset
Condenser, 7 reset return tank, 8 washing kettles, 9 ring body storage tanks, 10D3Tower, 11D3Condenser, 12D3Tower reboiler, 13D3Reflux
Tank, 14 product towers, 15 product tower condensers, 16 product tower reboilers, 17DMC storage tanks, 18 product reflux tanks
Specific implementation mode
Embodiment 1
30000 tons/year of diformazan hydrolysate heat drive circulation type cracking still
When the heat of the present invention drives circulation type cracking still as 30,000 tons/year of diformazan hydrolysates cracking, 1 ton of hydrolysate needs 0.4
Ton steam, hydrolysate：50%KOH solution (volume)=1：0.01, product purity：D4>=99.5%, DMC (D4+D5)≥
86.5%, need heat exchange area 80m through heat accounting2, the size of spiral heat exchangerIts structure is shown in figure
1, Fig. 2.
After diformazan hydrolysate is preheated and the mixture of KOH solution enters cracking still by lower part feed inlet 106, passes through liquid
104 top nozzle of distributor enters in corresponding cracking channel 122 to be mixed with solvent naphtha, and heat, side are absorbed from heat exchanger channels 121
Border ring vaporizes, and bubble, which rises, drives the liquid in cracking channel to rise to 122 top of cracking channel, after gas-liquid separation, solvent
Oily, unreacted organosilicon hydrolyzation object and KOH solution drop to cracker bottom by annular space, form Natural Circulation.Cyclisation
Gas after rearrangement after demister 102 further removal solvent naphtha by the gaseous phase outlet on cracking still top by being discharged.
The present invention the course of work be：
The hydrolysate preheated through hydrolysate heater 2 is mixed into heat with KOH solution and drives circulation type cracking still 3 in proportion,
Carry out catalytic cracking reaction under the action of heat carrier solvent naphtha, the gas after cyclisation is reset is directly entered cleavage column 5, in tower reactor
Wire body return heat drive circulation type cracking still, tower top ring body through rearrangement condenser 6 condense, be sent into purification system in washing kettle
8, D is entered after desalted water purification and washing3Tower 10, overhead vapours is through D3Condenser 11 is produced after condensing by certain reflux ratio, through pump
It is sent into hydrolysate tank 1, tower reactor liquid is delivered to product tower 14, and overhead vapours is after the condensation of product tower condenser 15 by certain reflux
Than extraction, it is sent into finished product D4Storage tank, lateral line discharging is DMC in tower, is sent into DMC storage tanks, and tower reactor epipodium returns after delivery pump pressurizes
Return hydrolysate tank 1.The cracking slag that heat is driven in circulation type cracking still is discharged through floss hole, is sent to out-of-bounds buried.
Embodiment 2
5.5 ten thousand tons/year of diformazan hydrolysate heat drive circulation type cracking still
When the heat of the present invention drives circulation type cracking still as 5.5 ten thousand tons/year of diformazan hydrolysates cracking, 1 ton of hydrolysate needs
0.392 ton of steam, hydrolysate：50%KOH solution (volume)=1：0.009, product purity：D4>=99.5%, DMC (D4+D5)≥
86.7%, need heat exchange area 150m through heat accounting2, the size of spiral heat exchangerIts structure is shown in figure
1, Fig. 2.
After diformazan hydrolysate is preheated and the mixture of KOH solution enters cracking still by lower part feed inlet 106, passes through liquid
104 top nozzle of distributor enters in corresponding cracking channel 122 to be mixed with solvent naphtha, and heat, side are absorbed from heat exchanger channels 121
Border ring vaporizes, and bubble, which rises, drives the liquid in cracking channel to rise to 122 top of cracking channel, after gas-liquid separation, solvent
Oily, unreacted organosilicon hydrolyzation object and KOH solution drop to cracker bottom by annular space, form Natural Circulation.Cyclisation
Gas after rearrangement after demister 102 further removal solvent naphtha by the gaseous phase outlet on cracking still top by being discharged.
The present invention the course of work be：
The hydrolysate preheated through hydrolysate heater 2 is mixed into heat with KOH solution and drives circulation type cracking still 3 in proportion,
Carry out catalytic cracking reaction under the action of heat carrier solvent naphtha, the gas after cyclisation is reset is directly entered cleavage column 5, in tower reactor
Wire body return heat drive circulation type cracking still, tower top ring body through rearrangement condenser 6 condense, be sent into purification system in washing kettle
8, D is entered after desalted water purification and washing3Tower 10, overhead vapours is through D3Condenser 11 is produced after condensing by certain reflux ratio, through pump
It is sent into hydrolysate tank 1, tower reactor liquid is delivered to product tower 14, and overhead vapours is after the condensation of product tower condenser 15 by certain reflux
Than extraction, it is sent into finished product D4Storage tank, lateral line discharging is DMC in tower, is sent into DMC storage tanks, and tower reactor epipodium returns after delivery pump pressurizes
Return hydrolysate tank 1.The cracking slag that heat is driven in circulation type cracking still is discharged through floss hole, is sent to out-of-bounds buried.
Comparative example 3
30000 tons/year of diformazan hydrolysate stirring-type cracking stills
The common outer stirring-type cracking still for having chuck, inside to carry heating coil is split as 30,000 tons/year of diformazan hydrolysates
Xie Shi, 1 ton of hydrolysate need 0.42 ton of steam, hydrolysate：50%KOH solution (volume)=1：0.011, product purity：D4≥
99%, DMC (D4+D5) >=85%.
It is found by the comparison of comparative example and embodiment 1-2, heat drives circulation type cracking still heat transfer efficiency height, reduces alkaline consumption
Amount, improves ring body yield and D4, DMC quality.
Claims (10)
1. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method of circulation, it is characterised in that：It is coaxial in the middle part of cracker
The double helix channel of class spiral-plate heat exchanger form is set, and helical duct upper and lower ends are not close one of in double helix channel
Envelope, as cracking channel, the sealing of another helical duct upper and lower ends forms heat exchanging medium passage, solvent naphtha in cracking channel and
It is distributed in annular space between the cylinder and cracker of double helix channel composition, the mixture of organosilicon hydrolyzation object and KOH solution is sent
Enter to crack in channel, the heat transferring mediums of heat exchanger channels provides heat for cracking channel, organosilicon hydrolyzation object in cracking channel with
Solvent naphtha mixes, the vaporization of side border ring, and bubble, which rises, drives the liquid in cracking channel to rise to cracking channel roof, gas-liquid point
From rear, solvent naphtha, unreacted organosilicon hydrolyzation object and KOH solution drop to cracker bottom by annular space, form nature
Cycle.
2. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method of circulation as described in claim 1, it is characterised in that：Cracking
Liquid distribution trough is arranged in bottom of device, by liquid distribution trough that organosilicon hydrolyzation object is corresponding with the mixture of KOH solution feeding
Cracking channel in.
3. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method of circulation as described in claim 1, it is characterised in that：Reaction
Afterwards, gas-liquid is discharged after the gas removal solvent naphtha isolated by cracker gas outlet in cracking channel roof separation.
4. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object cleavage method of circulation as described in claim 1, it is characterised in that：Cracking
Inverted cone segment and floss hole is arranged in bottom of device, reacts the cracking slag of generation in inverted cone segment after gravitational settling, gives from floss hole
Discharge.
5. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object cracker of circulation, it is characterised in that：Cracker include feed inlet,
Gas outlet, heat transferring medium entrance, heat transferring medium outlet, solvent oil-in, floss hole, feed inlet are arranged in cracker lower part one
Side, gas outlet setting are being split in cracker top center, heat transferring medium entrance, heat transferring medium outlet, the setting of solvent oil-in
Device top is solved, floss hole is arranged in cracker bottom centre；Class spiral-plate heat exchanger shape is coaxially disposed in the middle part of cracker
The double helix channel of formula, helical duct upper and lower ends blow-by one of in double helix channel are another as cracking channel
Helical duct upper and lower ends seal, and form heat exchanging medium passage, solvent naphtha is in cracking channel and the cylinder of double helix channel composition
Be distributed in annular space between cracker, feed inlet top be arranged liquid distribution trough, liquid distribution trough by organosilicon hydrolyzation object with
The mixture of KOH solution is sent into cracking channel.
6. a kind of solvent naphtha heat as claimed in claim 5 drives the organosilicon hydrolyzation object cracker of circulation, it is characterised in that：It splits
Solution device includes top seal head section, middle part cylindrical section and bottom inverted cone segment, and double helix channel is arranged in middle part cylindrical section, and with circle
Shell of column is coaxial；Preferably, demister is set between middle part cylindrical section and top seal head section.
7. a kind of solvent naphtha heat as claimed in claim 5 drives the organosilicon hydrolyzation object cracker of circulation, it is characterised in that：Liquid
Body distributor is made of coil pipe, and fluid injector is arranged on coil pipe, and nozzle vertically upward, or is arranged and is inserted upwardly into the vertical of cracking channel
Pipe, corresponding cracking channel, realizes that liquid is uniformly distributed.
8. a kind of solvent naphtha heat as claimed in claim 5 drives the organosilicon hydrolyzation object cracker of circulation, it is characterised in that：
It bores section bottom and floss hole is set.
9. a kind of solvent naphtha heat drives the organosilicon hydrolyzation object continuous cracking system of circulation, it is characterised in that：Including sequentially connected
Hydrolysate heater, cracker, cleavage column, rearrangement condenser, washing kettle, D as described in claim 5-8 is any3Tower, hydrolysis
Object tank, product tower, D4Storage tank, cleavage column tower reactor side line connect cracker, and condenser, D are reset in tower top connection3Column overhead connects
D3Condenser connects hydrolysate tank, D through pump3Tower connects product tower, and product column overhead connects product tower condenser, and connects finished product
D4Storage tank, product tower side line connect DMC storage tanks, and product tower tower reactor connects hydrolysate tank through pump.
10. a kind of method that solvent naphtha heat drives the organosilicon hydrolyzation object continuous cracking of circulation, it is characterised in that：Step is：
The organosilicon hydrolyzation object preheated through hydrolysate heater is mixed into proportion with KOH solution as claim 4-7 is any
The cracker, carries out catalytic cracking reaction under the action of heat carrier solvent naphtha, and the gas after cyclisation is reset is directly entered
Cleavage column, the wire body in tower reactor return cracking still, and tower top ring body is by resetting condenser condensation, the washing being sent into purification system
Kettle enters D after desalted water purification and washing3Tower, overhead vapours is through D3It produces, is pumped up by certain reflux ratio after condenser condensation
Entering hydrolysate tank, tower reactor liquid is delivered to product tower, and overhead vapours is produced after the condensation of product tower condenser by certain reflux ratio,
It is sent into finished product D4Storage tank, lateral line discharging is DMC in tower, is sent into DMC storage tanks, and tower reactor epipodium returns to hydrolysate after delivery pump pressurizes
Tank；Cracking slag in cracker is discharged through floss hole, is sent to out-of-bounds buried.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810450308.4A CN108409780B (en) | 2018-05-11 | 2018-05-11 | Method and device for cracking organic silicon hydrolysate by solvent oil thermal flooding circulation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810450308.4A CN108409780B (en) | 2018-05-11 | 2018-05-11 | Method and device for cracking organic silicon hydrolysate by solvent oil thermal flooding circulation |
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| CN108409780B CN108409780B (en) | 2020-06-16 |
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| Application Number | Title | Priority Date | Filing Date |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253429A (en) * | 2020-02-27 | 2020-06-09 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device and method for organic silicon cracking high ring and application |
| CN111875800A (en) * | 2020-06-30 | 2020-11-03 | 鲁西化工集团股份有限公司硅化工分公司 | Organosilicon pyrolysis residue recovery system and process and organosilicon production system |
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| CN111253429A (en) * | 2020-02-27 | 2020-06-09 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device and method for organic silicon cracking high ring and application |
| CN111253429B (en) * | 2020-02-27 | 2023-06-27 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device, method and application of organosilicon cracking high ring |
| CN111875800A (en) * | 2020-06-30 | 2020-11-03 | 鲁西化工集团股份有限公司硅化工分公司 | Organosilicon pyrolysis residue recovery system and process and organosilicon production system |
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| CN108409780B (en) | 2020-06-16 |
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