CN108358962A - A kind of method for continuously synthesizing of methyl sesquialter aluminium - Google Patents
A kind of method for continuously synthesizing of methyl sesquialter aluminium Download PDFInfo
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- CN108358962A CN108358962A CN201810331923.3A CN201810331923A CN108358962A CN 108358962 A CN108358962 A CN 108358962A CN 201810331923 A CN201810331923 A CN 201810331923A CN 108358962 A CN108358962 A CN 108358962A
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- aluminium
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 91
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000004411 aluminium Substances 0.000 title claims abstract description 79
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 43
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000003860 storage Methods 0.000 claims abstract description 15
- 230000004913 activation Effects 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 4
- OKJPEAGHQZHRQV-UHFFFAOYSA-N Triiodomethane Natural products IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 21
- 239000000463 material Substances 0.000 description 17
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- IAJOBQBIJHVGMQ-UHFFFAOYSA-N 2-amino-4-[hydroxy(methyl)phosphoryl]butanoic acid Chemical compound CP(O)(=O)CCC(N)C(O)=O IAJOBQBIJHVGMQ-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000006073 displacement reaction Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- 229940050176 methyl chloride Drugs 0.000 description 4
- 238000010923 batch production Methods 0.000 description 3
- CDPKWOKGVUHZFR-UHFFFAOYSA-N dichloro(methyl)phosphane Chemical compound CP(Cl)Cl CDPKWOKGVUHZFR-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- MCZQGJXPPZHLTG-UHFFFAOYSA-N C.[Cl] Chemical compound C.[Cl] MCZQGJXPPZHLTG-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 244000037671 genetically modified crops Species 0.000 description 2
- 230000002363 herbicidal effect Effects 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 125000001340 2-chloroethyl group Chemical class [H]C([H])(Cl)C([H])([H])* 0.000 description 1
- 239000005561 Glufosinate Substances 0.000 description 1
- 239000005562 Glyphosate Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- HYZXMVILOKSUKA-UHFFFAOYSA-K chloro(dimethyl)alumane;dichloro(methyl)alumane Chemical compound C[Al](C)Cl.C[Al](Cl)Cl HYZXMVILOKSUKA-UHFFFAOYSA-K 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 1
- 229940097068 glyphosate Drugs 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000009261 transgenic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/064—Aluminium compounds with C-aluminium linkage compounds with an Al-Halogen linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method for continuously synthesizing of methyl sesquialter aluminium, activation suspension is formed with aluminium powder, initiator and solvent, in continuous conveying to synthetic tower, the chloromethanes counter current contacting reaction in synthetic tower and being continuously passed through, the methyl sesquialter aluminum solutions of generation are collected in storage tank after cooling by bottom of tower, and the raw material of other products is used for as finished product.This have the advantage that safety, equipment is few, and yield is big.
Description
Technical field
The present invention relates to technical field of fine, more particularly to a kind of method for continuously synthesizing of methyl sesquialter aluminium.
Background technology
Methyl sesquialter aluminium is also known as sesquialter methyl chloride aluminium, English name Methylaluminum sesquichloride,
CAS 12542-85-7, solid-state are white or yellowish crystallization, and liquid is micro- yellow liquor body, 23 DEG C of fusing point.Molecular formula：
C3H9Al2Cl3。
It is the primary raw material for preparing the compounds such as trimethyl aluminium, dichloromethylphosphine.It is poly- that trimethyl aluminium is widely used in alkene
The industries such as conjunction, photoelectricity, and dichloromethylphosphine can be used for manufacturing fire retardant, herbicide glufosinate-ammonium and other pesticides, medicine etc.
Synthesis.
Methyl sesquialter aluminium then can be used for preparing dichloromethylphosphine, be the important intermediate for synthesizing glufosinate-ammonium.Glufosinate-ammonium
(glufosinate) it is novel steriland herbicide that Hirst company develops the eighties in last century, can be used for orchard, Portugal
1 year and perennial dicotyledonous and grassy weed are prevented and kill off in grape garden, bare place.Hirst company is using glufosinate-ammonium as target, by anti-
Property gene transfer, selection and breeding resistant crop varieties, have successfully imported rice, wheat, corn etc. 20 by the resistant gene of glufosinate-ammonium
In various crop.These genetically modified crops are not only generally planted in north America region, in recent years in parts such as Asia, Australia, Europe
Countries and regions also begin to promote, and glufosinate-ammonium dosage is only second to glyphosate at present, are that second-biggest-in-the-world genetically modified crops tolerance removes
Careless agent.With the high speed development of transgenic technology and quitting listing for large-tonnage herbicides paraquat, the market prospects of glufosinate-ammonium are very
It is good, therefore continuous synthesizing methyl sesquialter aluminium method makes great sense.
The method of synthesizing methyl sesquialter aluminium is high pressure batch process at present, and that there are equipment is more for batch process production, leakage point is more, endangers
It is big to invest more, high energy consumption, risk for the shortcomings such as danger point is more, efficiency is low when large-scale production produces.
Invention content
The present invention provides a kind of method for continuously synthesizing of methyl sesquialter aluminium aiming at above-mentioned defect.The present invention
It is that activation suspension is formed with aluminium powder, initiator and solvent, in continuous conveying to synthetic tower, in synthetic tower and is continuously passed through
Chloromethanes counter current contacting is reacted, and the methyl sesquialter aluminum solutions of generation are collected in storage tank after cooling by bottom of tower, is used as finished product
In the raw material of other products.Compared with the prior art, present device is few, and dangerous small, at low cost, low energy consumption, efficient.
A kind of method for continuously synthesizing technical solution of methyl sesquialter aluminium of the present invention is, with aluminium powder, initiator and solvent shape
At activation suspension, in continuous conveying to synthetic tower, the chloromethanes counter current contacting reaction in synthetic tower and being continuously passed through generates
Methyl sesquialter aluminum solutions be collected in storage tank after cooling by bottom of tower, as finished product be used for other products raw material.
A kind of method for continuously synthesizing of methyl sesquialter aluminium, includes the following steps：
（1）Aluminium powder suspension preparation activates：Aluminium powder, initiator, solvent are continuously put into blending tank, be stirred and cause shape
At runny suspension；
（2）Methyl sesquialter aluminum solutions continuously synthesize：Suspension after activation is continuously introduced at the top of synthetic tower, under free flow, with tower
The chloromethanes counter current contacting that lower part is continuously passed through, reaction generate methyl sesquialter aluminum solutions and are flowed out from synthetic tower bottom；
（3）Product cools down：The methyl sesquialter aluminum solutions cooling without aluminium powder of bottom of tower outflow；
（4）Product after cooling enters storage tank.
Step（1）In, the fineness of aluminium powder is not less than 400 mesh, and content is not less than 98%, and moisture is not more than 0.05%.
Step（1）In, the weight ratio of aluminium powder and solvent is 1:4.0-20.0 preferably 1:12—18.0；Aluminium powder and initiator
Weight ratio be 100:0.1-1.0, preferably 100: 0.5.
Step（1）In, it is 50 DEG C -80 DEG C to be stirred temperature, preferably 70 DEG C, is stirred time 20-60min, preferably
30min。
Step（1）In, initiator is at least one of methyl sesquialter aluminium, iodine, iodomethane, bromomethane；Solvent is methyl
At least one of sesquialter aluminium, saturated alkane, ethers, aromatic hydrocarbon.Initiator and the preferred methyl sesquialter aluminium ontology of solvent, product
For one-component, it is conducive to follow-up use.
Step（2）In, the feeding temperature of synthetic tower is kept for 50-80 DEG C, and drop temperature is not more than 135 DEG C.
Step（2）The molar ratio of middle aluminium powder and chloromethanes is 1.0:1.5-2.0.
Step（2）In, synthesis tower top blow-down pipe has fluid-tight protection, and has small-range flowmeter to detect excessive chloromethanes.
After normal operation, the weight of synthetic tower bottom discharging is that the sum of two kinds of inlet amounies subtract the amount that chloromethanes is discharged in synthetic tower blow-down pipe
Difference do not submerge chloromethanes to ensure that materials at bottom of tower neither flows sky yet and ventilate into tower mouth.
Aluminium powder suspension and chloromethanes enter before synthetic tower through accurate metering, and bottom of tower discharging also must be measured accurately, with kg/
H is measured.
1 step（3）In, the product temperatur after cooling is 30 DEG C -60 DEG C；
Step（4）In, 30 DEG C -50 DEG C of product reservoir temperature.
A kind of method for continuously synthesizing flow of methyl sesquialter aluminium of the present invention is as follows：
（1）After aluminium powder is first prepared activation system progress nitrogen displacement deoxygenation and water, then under nitrogen protection into blending tank
Quantitative aluminium powder, initiator and solvent is added, keep the temperature and is stirred, for use.
（2）Synthesis, cooling, stocking system are thoroughly replaced with nitrogen, 90 DEG C of thermostatic medium is passed through to synthesis tower casing journey
And keep synthetic tower temperature constant, and chloromethanes is passed through by tower lower gas entrance, after having methyl chloride gas spilling in tower top fluid-tight,
By for use aluminium powder suspension with being pumped at the top of synthetic tower, make two kinds of material counter current contactings, adjust the flow of two kinds of materials, protects
The micro- excess of chloromethanes is held, while adjusting tower temperature, so that bottom discharge temperature is not more than 135 DEG C, control tower bottom discharging flow ensures
There is fluid-tight in expects pipe, in case chloromethanes is overflowed by bottom of tower with product.After system normal operation, from feeder to aluminium powder suspension tank
In be continuously added to aluminium powder, while initiator and solvent are proportionally added into, to form continuous production.
（3）After the methyl sesquialter aluminium discharging of synthesis, heat exchanger cooling medium consumption is adjusted, the object flowed out by heat exchanger is controlled
Material temperature degree flows into product storage tank at 30 DEG C -60 DEG C.
（4）Product transfering material pump or nitrogen in storage tank, which are sent into, uses post, forms continuous production.
In addition, the method for the present invention is also applied for ethyl sesquialter aluminium (C2H5)3Al2Cl3Continuous synthesis, with aluminium powder, initiator
Activation suspension is formed with solvent, in continuous conveying to synthetic tower, the chloroethanes counter current contacting that in synthetic tower and is continuously passed through
Reaction generates ethyl sesquialter aluminum solutions.
Beneficial effects of the present invention are：This have the advantage that safety, equipment is few, and yield is big.High pressure batch process is given birth to
It produces, is first stood after every batch of aluminium powder charging, wait for that aluminium powder dust settling is complete, need vacuum, nitrogen displacement twice, then chloromethanes displacement two
Secondary, the time is longer；And during the reaction, since jacket for heat exchange area is small, the removal of reaction heat is limited, the intake of chloromethanes
It is limited, so that production efficiency is reduced；After reaction, temperature of charge is at 120-135 DEG C, and cooling still needs to the long period, feed intake,
In the links such as displacement, it is susceptible to error, air or moisture is caused to enter, generates security risk, and reaction later stage is higher,
There is also certain risks.
This patent method is normal pressure production, and absorption tower heat exchange area is big, and heat removes immediately, after product leaves synthetic tower
Cool down in time through heat exchanger, so efficiency is higher, safety is preferable.
The daily yield of prior art 2000L reaction kettles is the pure methyl sesquialter aluminium of 1500L, needs 300kg aluminium powders, and with originally
Inventive method can produce 6000L daily, need aluminium powder 1200kg, so equipment is few under same production scale, yield is big.Interval is high
Platen press production needs higher reaction pressure, there is certain danger.
Description of the drawings：
Fig. 1 show the method for the present invention device therefor schematic diagram.
In figure, 1- blending tanks, 2- synthetic towers, 3- heat exchangers, 4- storage tanks, 5- pumps.
Specific implementation mode：
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but it is of the invention
It is not limited thereto.
Embodiment 1
A kind of method for continuously synthesizing of methyl sesquialter aluminium：Nitrogen displacement is carried out to production system, it is ensured that air is thoroughly replaced.To
100kg aluminium powders, 0.5kg iodine and 1500kg dimethylbenzene are added in blending tank 1, stirring is warming up to 70 DEG C, activates 30 min.
Synthetic tower 2, heat exchanger 3, finished product storage tank 4 are carried out nitrogen thoroughly to replace, it is ensured that anaerobic is anhydrous in system.
It is passed through heat transferring medium to synthetic tower 2, so that temperature in tower is kept for 90 DEG C, is passed through chloromethanes, waits for that drain has chloromethanes
Outflow, while aluminium powder is activated into suspension material with pump 5 and is sent into 2 tower top of synthetic tower, the flow for adjusting aluminium powder activation suspension material is
400kg/h, chloromethanes flow are 80 kg/h.The temperature and flow velocity for adjusting 2 heat transferring medium of synthetic tower, make bottom of tower drop temperature exist
120-125℃。
Adjusting discharging flow is 480kg/h, while adjusting heat exchanger 3 and cooling down medium, makes temperature of charge at 30-60 DEG C, and
Material is set to enter storage tank 4.
After material continuous operation, aluminium powder 25kg/h, 0.125kg/h iodine and 375kg/h diformazans are continuously added into blending tank 1
Benzene, while activation temperature is kept, and keep the stability of flow of delivery pump 5.
The prior art produces 10000 tons of methyl sesquialter aluminium and needs equipment：2000L autoclaves 20,20 sets of aluminium powder charging dresses
It sets, 20 sets of mating logical methyl chloride system（Containing metering, control, all kinds of instrument, valve, pipeline etc.）, employment is more, and leakage point is more,
Plant maintenance heavy workload, high energy consumption.
And the film-falling absorption tower of 1 200 squares of this method needs, 1 set of logical methyl chloride system, 1 set of aluminium powder charging device,
Equipment is few under same production scale, and yield is big.
Embodiment 2
A kind of method for continuously synthesizing of methyl sesquialter aluminium：Nitrogen displacement is carried out to system, it is ensured that air is thoroughly replaced.To mixing
100kg aluminium powders, 0.5kg iodine and 2000kg dimethylbenzene are added in tank 1, stirring is warming up to 60 DEG C, activates 40 min.
Synthetic tower 2, heat exchanger 3, finished product storage tank 4 are carried out nitrogen thoroughly to replace, it is ensured that anaerobic is anhydrous in system.
It is passed through heat transferring medium to synthetic tower 2, so that temperature in tower is kept for 90 DEG C, is passed through chloromethanes, waits for that drain has chloromethanes
Outflow, while aluminium powder is activated into suspension material with pump 5 and is sent into tower top, the flow for adjusting aluminium powder activation suspension material is 1050kg/h, chlorine
Methane flow is 150 kg/h.The temperature and flow velocity for adjusting 2 heat transferring medium of synthetic tower, make bottom of tower drop temperature 120-125
℃。
Adjusting discharging flow is 1190kg/h, while adjusting heat exchanger 3 and cooling down medium, makes temperature of charge at 30-60 DEG C, and
Material is set to enter storage tank 4.
After material continuous operation, aluminium powder 50kg/h, 0.25kg/h iodine and 1000kg/h diformazans are continuously added into blending tank 1
Benzene, while activation temperature is kept, and keep the stability of flow of delivery pump 5.
Embodiment 3
A kind of method for continuously synthesizing of methyl sesquialter aluminium：Nitrogen displacement is carried out to system, it is ensured that air is thoroughly replaced.To mixing
100kg aluminium powders and 2000kg methyl sesquialter aluminium products are added in tank 1, stirring is warming up to 60 DEG C, activates 40 min.
Synthetic tower 2, heat exchanger 3, finished product storage tank 4 are carried out nitrogen thoroughly to replace, it is ensured that anaerobic is anhydrous in system.
It is passed through heat transferring medium to synthetic tower 2, so that temperature in tower is kept for 90 DEG C, is passed through chloromethanes, waits for that drain has chloromethanes
Outflow, while aluminium powder is activated into suspension material with pump 5 and is sent into tower top, the flow for adjusting aluminium powder activation suspension material is 1050kg/h, chlorine
Methane flow is 150 kg/h.The temperature and flow velocity for adjusting 2 heat transferring medium of synthetic tower, make bottom of tower drop temperature at 120-125 DEG C.
Adjusting discharging flow is 1190kg/h, while adjusting heat exchanger 3 and cooling down medium, makes temperature of charge at 30-60 DEG C, and
Material is set to enter storage tank 4.
After material continuous operation, aluminium powder 50kg/h and 1000kg/h methyl sesquialter aluminum solutions are continuously added into blending tank 1,
Activation temperature is kept simultaneously, and keeps the stability of flow of delivery pump 5.
Claims (10)
1. a kind of method for continuously synthesizing of methyl sesquialter aluminium, which is characterized in that form activation with aluminium powder, initiator and solvent and suspend
Liquid, in continuous conveying to synthetic tower, the chloromethanes counter current contacting reaction in synthetic tower and being continuously passed through, the methyl sesquialter of generation
Aluminum solutions are collected in storage tank after cooling by bottom of tower, and the raw material of other products is used for as finished product.
2. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 1, which is characterized in that including following step
Suddenly：
（1）Aluminium powder suspension preparation activates：Aluminium powder, initiator, solvent are continuously put into blending tank, be stirred and cause shape
At runny suspension；
（2）Methyl sesquialter aluminum solutions continuously synthesize：Suspension after activation is continuously introduced at the top of synthetic tower, under free flow, with tower
The chloromethanes counter current contacting that lower part is continuously passed through, reaction generate methyl sesquialter aluminum solutions and are flowed out from synthetic tower bottom；
（3）Product cools down：The methyl sesquialter aluminum solutions cooling without aluminium powder of bottom of tower outflow；
（4）Product after cooling enters storage tank.
3. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（1）In, aluminium
The fineness of powder is not less than 400 mesh, and content is not less than 98%, and moisture is not more than 0.05%.
4. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（1）In, aluminium
The weight ratio of powder and solvent is 1:4.0-20.0；The weight ratio of aluminium powder and initiator is 100:0.1-1.0.
5. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（1）In, it stirs
It is 50 DEG C -80 DEG C to mix mixing temperature, is stirred time 20-60min.
6. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（1）In, draw
Hair agent is at least one of methyl sesquialter aluminium, iodine, iodomethane, bromomethane；Solvent be methyl sesquialter aluminium, saturated alkane, ethers,
At least one of aromatic hydrocarbon.
7. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（2）In, it closes
Kept for 50-80 DEG C at the feeding temperature of tower, drop temperature is not more than 135 DEG C.
8. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（2）Middle aluminium
The molar ratio of powder and chloromethanes is 1.0:1.5-2.0.
9. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（2）In, just
Often operation after, synthetic tower bottom discharging weight be the sum of two kinds of inlet amounies subtract in synthetic tower blow-down pipe be discharged chloromethanes amount it
Difference.
10. a kind of method for continuously synthesizing of methyl sesquialter aluminium according to claim 2, which is characterized in that step（3）In,
Product temperatur after cooling is 30 DEG C -60 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183486A (en) * | 2019-06-10 | 2019-08-30 | 山东亿盛实业股份有限公司 | It is a kind of to mediate the method and production system for squeezing out continuous synthesizing methyl dichloride phosphine |
| CN112480158A (en) * | 2020-12-31 | 2021-03-12 | 江苏爱姆欧光电材料有限公司 | Continuous production process of aluminum sesquiethylate chloride |
| CN112480159A (en) * | 2020-12-31 | 2021-03-12 | 江苏爱姆欧光电材料有限公司 | Continuous production process of sesquimethyl aluminum chloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110183486A (en) * | 2019-06-10 | 2019-08-30 | 山东亿盛实业股份有限公司 | It is a kind of to mediate the method and production system for squeezing out continuous synthesizing methyl dichloride phosphine |
| CN110183486B (en) * | 2019-06-10 | 2021-06-29 | 山东亿盛实业股份有限公司 | Method for kneading and extruding to continuously synthesize methyl phosphine dichloride and production system |
| CN112480158A (en) * | 2020-12-31 | 2021-03-12 | 江苏爱姆欧光电材料有限公司 | Continuous production process of aluminum sesquiethylate chloride |
| CN112480159A (en) * | 2020-12-31 | 2021-03-12 | 江苏爱姆欧光电材料有限公司 | Continuous production process of sesquimethyl aluminum chloride |
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Denomination of invention: A continuous synthesis method of methyl sesquial Effective date of registration: 20220526 Granted publication date: 20200721 Pledgee: Jinxiang County sub branch of Postal Savings Bank of China Ltd. Pledgor: SHANDONG YISHENG INDUSTRIAL CO.,LTD. Registration number: Y2022980006388 |