CN107141234A - A kind of azo-bis-iso-dimethyl synthetic method - Google Patents
A kind of azo-bis-iso-dimethyl synthetic method Download PDFInfo
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- CN107141234A CN107141234A CN201610526787.4A CN201610526787A CN107141234A CN 107141234 A CN107141234 A CN 107141234A CN 201610526787 A CN201610526787 A CN 201610526787A CN 107141234 A CN107141234 A CN 107141234A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C245/00—Compounds containing chains of at least two nitrogen atoms with at least one nitrogen-to-nitrogen multiple bond
- C07C245/02—Azo compounds, i.e. compounds having the free valencies of —N=N— groups attached to different atoms, e.g. diazohydroxides
- C07C245/04—Azo compounds, i.e. compounds having the free valencies of —N=N— groups attached to different atoms, e.g. diazohydroxides with nitrogen atoms of azo groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
Abstract
The invention discloses a kind of azo-bis-iso-dimethyl synthetic method, comprise the steps：（1）Condensation：Azodiisobutyronitrile, methanol, isophorone are added in reaction vessel, phosphorus trichloride solution is added and is reacted, centrifugation obtains azoimide methyl ether hydrochloride solid material；（2）Hydrolysis：Pure water is added in hydrolysis vessels, azoimide methyl ether hydrochloride solid material is added to hydrolysis vessels and is hydrolyzed；（3）Split-phase：Feed liquid after hydrolysis is put into split-phase container, split-phase is carried out with consisting of phase-transferring agent hexadecyltrimethylammonium chloride；（4）Recrystallization；（5）Dry.The present invention is by designing process route and feedstock optimization, and raw material is environment-protecting and non-poisonous, and reacting balance is easily-controllable, substantially increases the security of reaction；Product separation is more thorough, greatly improves product yield；Discharge of wastewater is reduced, effectively alleviates environmental protection pressure；Reaction time is short, and energy consumption is low, substantially reduces production cost.
Description
Technical field
The present invention relates to a kind of azo-bis-iso-dimethyl synthetic method, belong to chemosynthesis technical field.
Background technology
POP full name grafted polyether polyols, abbreviation graft polyether is that the compound of vinyl-containing monomers is grafted in polyethers
A kind of polymer that copolymerization is obtained, the polyurethane foam produced with it has higher bearing capacity and good resilience
Energy.Developed country's graft polyether yield accounts for more than the 1/5 of general polyethers.China was continuously increased to POP demand in recent years.But
In POP production process, the property of initiator and its analyte can directly affect the production technology and products characteristics of polymer.
Conventional polymerization initiator azodiisobutyronitrile（AIBN）After decomposition, its product is hypertoxic solid-state tetramethyl succinonitrile, in monomer
It can not be dissolved with polymer, cause POP to produce the problem of generally existing easily blocks pipeline.Meanwhile, with polyethers industry competition
Be growing more intense, the normal starter such as AIBN is also far from meeting product requirement.
Azo-bis-iso-dimethyl（AIBME）Have the advantages that its is unique as novel azo compound initiator of birdsing of the same feather flock together：Trigger and live
Property is moderate, and polymerisation is easily controlled.It is not only nontoxic, decompose not blocked pipeline, and product can also be improved during steady, use
Quality and conversion ratio.Make initiator polymerization with AIBME and obtain POP, product colour is more shallow, and feel is more comfortable.AIBME not only may be used
To substitute AIBN completely, and final using effect is better than AIBN.Domestic several main POP manufacturers use instead in succession
AIBME, in polymer polyol alcohol production, using AIBME as initiator, can be such that the quality of polymer polyatomic alcohol substantially carries
Height, viscosity drops to 3,000 4000 mPas, and monomer mass fraction is down to less than 100 × 1016.And product residue monomer
Few, more stable in storage and transport process, not stratified, conversion rate of products also improves 1% or so, can effectively reduce integrated cost.
Azo-bis-iso-dimethyl（AIBME）Traditional synthesis mainly has two methods：One is with AIBN, methanol, first
Benzene and anhydrous hydrogen chloride are raw material, and such as 164 g (1 mo1) AIBN and 76.8 g (2.4 mo1) methanol is in 800 mL toluene solvants
Middle stirring at normal temperature, is passed through 110 g (3 mo1) anhydrous hydrogen chloride and reacts 16 h, generate azo imino-ethers hydrochloride intermediate, gained
Azo imido ether hydrochloride be hydrolyzed with 500 mL water obtain target product again, final sterling AIBME about 170g.
Another method be using chlorine, azodiisobutyronitrile hydrazine (HAIBN) and methanol as raw material, such as 166 g HAIBN and
76.8 g (2.4 mo1) methanol stirring at normal temperature in 800 mL toluene, is passed through the h of 74.6 g (1.05 mo1) chlorine reaction 20, raw
It is hydrolyzed again with 500 mL water into azo imino-ethers ammonia ether hydrochloride and obtains target product, the final g of sterling AIBME about 170.
Two methods synthetic route is long in traditional handicraft, and solvent for use is poisonous benzene class or halogenated aryl hydrocarbon, in human body and
Environmental hazard is very big.And need to be passed through chlorine or hydrogen chloride gas, reaction acutely is difficult to control, and often occurs emitting the safety such as kettle
Accident, still have after Hydrolysis of crude freezing it is a small amount of it is soluble in water be difficult to reclaim, yield is relatively low；Wastewater produced is highly acid, it is difficult to
Qualified discharge is handled, environmental protection pressure is very big, is not suitable for industrial-scale production.
The content of the invention
It is an object of the invention to overcome shortcoming present in prior art, the present invention provides a kind of isobutyric acid two of azo two
Methyl esters synthetic method, by designing process route and feedstock optimization, raw material is environment-protecting and non-poisonous, and reacting balance is easily-controllable, greatly improves
The security of reaction；Product separation is more thorough, greatly improves product yield；Discharge of wastewater is reduced, effectively alleviates environmental protection pressure；
Reaction time is short, and energy consumption is low, substantially reduces production cost.
The technical scheme is that：
A kind of azo-bis-iso-dimethyl synthetic method, comprises the steps：
（1）Condensation：Azodiisobutyronitrile, methanol, isophorone are added in reaction vessel, the lower addition phosphorus trichloride of stirring is molten
Liquid is reacted, and reaction is finished, and feed liquid is centrifuged, and obtains azoimide methyl ether hydrochloride solid material；
（2）Hydrolysis：Pure water is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride solid material is in stirring
Mix down and be added to hydrolysis vessels and be hydrolyzed；
（3）Split-phase：Feed liquid after hydrolysis is put into split-phase container, divided with consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；
（4）Recrystallization：Methanol solution addition crystallisation vessel is recrystallized, azo-bis-iso-dimethyl wet product is obtained；
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, room temperature≤25 DEG C are dried.
Step（1）Condensation step is：The azodiisobutyronitrile measured, methanol, isophorone are added to reaction vessel
It is interior, start stirring, insulation reaction 8-15 hours after phosphorus trichloride solution, 10-30 DEG C of reaction temperature, completion of dropping are added dropwise；Will material
Liquid is centrifuged, and obtains azoimide methyl ether hydrochloride solid material；Mass concentration >=95% of the phosphorus trichloride solution；It is above-mentioned
The mol ratio of raw material is azodiisobutyronitrile：Methanol：Isophorone：Phosphorus trichloride=1：2-3.5：3.2-5.8：2-2.8；
Step（2）Hydrolysing step is：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide first
Ether hydrochloride solid material is added to hydrolysis vessels with stirring, controls 10-30 DEG C of temperature, treats that azoimide methyl ether hydrochloride is added
Finish, regulation system pH value is hydrolyzed for 4-9；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：2-4.5.
Step（3）Split-phase step is：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is kept
At 18-22 DEG C, stand 2-4h and carry out split-phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent cetyl
The addition of trimethyl ammonium chloride is the 0.05-0.5 of hydrolyzation material volume.
Step（4）Re-crystallization step is：The methanol solution measured is added in crystallisation vessel, control temperature 20-25
DEG C, start slow cooling after organic phase is completely dissolved, temperature slows down cooling rate when being down to 10 DEG C, it was observed that in crystallisation vessel
When having crystal precipitation, slow down mixing speed, accelerate cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, be incubated growing the grain
1-3h, is then slowly put into centrifugation apparatus by feed liquid, and after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl
Wet product.
Step（4）The concentration of middle methanol solution is 65%；The consumption of methanol solution is 2.5-5.5 times of organic phase volume.
To achieve these goals, the present invention is first thrown azodiisobutyronitrile, methanol and isophorone by certain mol proportion
Enter in container, phosphorus trichloride solution be then added dropwise, control temperature is reacted, and obtains azoimide methyl ether hydrochloride, then by its
It is added to the water and reaction is hydrolyzed, consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added in system, direct split-phase obtains idol
The isobutyl dimethyl phthalate crude product of nitrogen two, crude product obtains azo-bis-iso-dimethyl sterling after recrystallization.
Compared with traditional synthesis, the invention has the advantages that：
（1）Traditional handicraft needs, with poisonous solvent such as toluene or halogenated aryl hydrocarbon, there is very big harm to human body and environment.This hair
Bright preferred through many experiments, selection isophorone is solvent, and its flash-point is high, safe, and its toxicity is very low, can effectively drop
The low harm to human body and environment, and can apply mechanically repeatedly.
（2）Improve feeding mode, traditional handicraft needs to be passed through chlorine or hydrogen chloride gas, reaction time length and whard to control
Temperature, overtemperature explosion hazard is big.The present invention is raw material from liquid phosphorus trichloride, can be by controlling its rate of addition to control
Reaction temperature processed, it is to avoid overtemperature explosion danger, reacting balance is easily controllable, and the reaction time greatly shortens, and effectively increases life
Produce efficiency.
（3）Reform operating unit, reduce energy resource consumption, improve yield.Azo-bis-iso-dimethyl is slightly soluble in water, tradition
Technique needs directly freezed to crystallize, and still has a small amount of azo-bis-iso-dimethyl to dissolve in its water, it is impossible to reclaim.This technique is by water
Solve and consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added in product system, azo-bis-iso-dimethyl can be made completely by aqueous phase
Organic phase is transferred to, is operated and separated by split-phase, effectively reduction cold energy consumption, simplifies production operation, improves product yield.
（4）Wastewater produced pH value is in 1-3 in traditional handicraft, and acidity is difficult to handle by force, and this technique waste water pH value is 6-7,
And water can be reduced to original 80%, effectively alleviate environmental protection pressure.
It is using the beneficial effect produced by above-mentioned technical proposal：
The present invention is by designing process route and feedstock optimization, and raw material is environment-protecting and non-poisonous, and reacting balance is easily-controllable, substantially increases anti-
The security answered；Product separation is more thorough, greatly improves product yield and purity；Discharge of wastewater is reduced, effectively alleviates environmental protection pressure
Power；Reaction time is short, and energy consumption is low, substantially reduces production cost.
Embodiment
The present invention is described in further detail with reference to embodiment.
Embodiment 1
（1）Condensation：The azodiisobutyronitrile measured, methanol, isophorone are added in reaction vessel, start stirring, drop
Plus phosphorus trichloride solution, 25 DEG C of reaction temperature, insulation reaction 8 hours after completion of dropping；Feed liquid is centrifuged, azo is obtained sub-
Amine methyl ether hydrochloride solid material；The mass concentration of phosphorus trichloride solution is 95%；The mol ratio of raw material is azodiisobutyronitrile：First
Alcohol：Isophorone：Phosphorus trichloride=1：2：3.2：2；
（2）Hydrolysis：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride is consolidated
Body material is added to hydrolysis vessels with stirring, controls 30 DEG C of temperature, treats that the addition of azoimide methyl ether hydrochloride is finished, regulation system
PH value is hydrolyzed for 6；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：2.
（3）Split-phase：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is maintained at 19 DEG C, quiet
Put 2h and carry out split-phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Addition is 0.2 times of hydrolyzation material volume.
（4）Recrystallization：The methanol solution measured is added in crystallisation vessel, 23 DEG C of temperature is controlled, treats that organic phase is complete
Start slow cooling after fully dissolved, temperature slows down cooling rate when being down to 10 DEG C, it was observed that when having crystal precipitation in crystallisation vessel,
Slow down mixing speed, accelerate cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, growing the grain 3h is incubated, then by feed liquid
Centrifugation apparatus slowly is put into, after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl wet product.Methanol solution
Concentration is 65%；The consumption of methanol solution is 3 times of organic phase volume.
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, azo-bis-iso-dimethyl dry product is obtained；It is dry
Dry room temperature≤25 DEG C.
Calculated yield is simultaneously tested to product, and the yield of azo-bis-iso-dimethyl is 94.5% in the present embodiment,
Product purity is 99.83%.
Embodiment 2
（1）Condensation：The azodiisobutyronitrile measured, methanol, isophorone are added in reaction vessel, start stirring, drop
Plus phosphorus trichloride solution, 10 DEG C of reaction temperature, insulation reaction 15 hours after completion of dropping；Feed liquid is centrifuged, azo is obtained
Imines methyl ether hydrochloride solid material；The mass concentration of the phosphorus trichloride solution is 97%；The mol ratio of raw material is the isobutyl of azo two
Nitrile：Methanol：Isophorone：Phosphorus trichloride=1：2：5.8：2.8；
（2）Hydrolysis：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride is consolidated
Body material is added to hydrolysis vessels with stirring, controls 20 DEG C of temperature, treats that the addition of azoimide methyl ether hydrochloride is finished, regulation system
PH value is hydrolyzed for 4；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：3.
（3）Split-phase：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is maintained at 20 DEG C, quiet
Put 4h and carry out split-phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Addition is 0.05 times of hydrolyzation material volume.
（4）Recrystallization：The methanol solution measured is added in crystallisation vessel, 22 DEG C of temperature is controlled, treats that organic phase is complete
Start slow cooling after fully dissolved, temperature slows down cooling rate when being down to 10 DEG C, it was observed that when having crystal precipitation in crystallisation vessel,
Slow down mixing speed, accelerate cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, growing the grain 1h is incubated, then by feed liquid
Centrifugation apparatus slowly is put into, after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl wet product.Methanol solution
Concentration is 65%；The consumption of methanol solution is 2.5 times of organic phase volume.
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, azo-bis-iso-dimethyl dry product is obtained；It is dry
Dry room temperature≤25 DEG C.
Calculated yield is simultaneously tested to product, and the yield of azo-bis-iso-dimethyl is 93.8% in the present embodiment,
Product purity is 99.45%.
Embodiment 3
（1）Condensation：The azodiisobutyronitrile measured, methanol, isophorone are added in reaction vessel, start stirring, drop
Plus phosphorus trichloride solution, 30 DEG C of reaction temperature, insulation reaction 10 hours after completion of dropping；Feed liquid is centrifuged, azo is obtained
Imines methyl ether hydrochloride solid material；The mass concentration of the phosphorus trichloride solution is 95%；The mol ratio of raw material is the isobutyl of azo two
Nitrile：Methanol：Isophorone：Phosphorus trichloride=1：3.5：5.8：2.8；
（2）Hydrolysis：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride is consolidated
Body material is added to hydrolysis vessels with stirring, controls 10 DEG C of temperature, treats that the addition of azoimide methyl ether hydrochloride is finished, regulation system
PH value is hydrolyzed for 7；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：4.
（3）Split-phase：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is maintained at 18 DEG C, quiet
Put 3h and carry out split-phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Addition is 0.5 times of hydrolyzation material volume.
（4）Recrystallization：The methanol solution measured is added in crystallisation vessel, 20 DEG C of temperature is controlled, treats that organic phase is complete
Start slow cooling after fully dissolved, temperature slows down cooling rate when being down to 10 DEG C, it was observed that when having crystal precipitation in crystallisation vessel,
Slow down mixing speed, accelerate cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, growing the grain 2h is incubated, then by feed liquid
Centrifugation apparatus slowly is put into, after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl wet product.Methanol solution
Concentration is 65%；The consumption of methanol solution is 4 times of organic phase volume.
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, azo-bis-iso-dimethyl dry product is obtained；It is dry
Dry room temperature≤25 DEG C.
Calculated yield is simultaneously tested to product, and the yield of azo-bis-iso-dimethyl is 94.8% in the present embodiment,
Product purity is 99.58%.
Embodiment 4
（1）Condensation：The azodiisobutyronitrile measured, methanol, isophorone are added in reaction vessel, start stirring, drop
Plus phosphorus trichloride solution, 20 DEG C of reaction temperature, insulation reaction 12 hours after completion of dropping；Feed liquid is centrifuged, azo is obtained
Imines methyl ether hydrochloride solid material；The mass concentration of phosphorus trichloride solution is 96%；The mol ratio of raw material is azodiisobutyronitrile：
Methanol：Isophorone：Phosphorus trichloride=1：3.5：3.2：2.8；
（2）Hydrolysis：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride is consolidated
Body material is added to hydrolysis vessels with stirring, controls 25 DEG C of temperature, treats that the addition of azoimide methyl ether hydrochloride is finished, regulation system
PH value is hydrolyzed for 9；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：4.5.
（3）Split-phase：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is maintained at 22 DEG C, quiet
Put 2.5h and carry out split-phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Addition be 0.3 times of hydrolyzation material volume.
（4）Recrystallization：The methanol solution measured is added in crystallisation vessel, 25 DEG C of temperature is controlled, treats that organic phase is complete
Start slow cooling after fully dissolved, temperature slows down cooling rate when being down to 10 DEG C, it was observed that when having crystal precipitation in crystallisation vessel,
Slow down mixing speed, accelerate cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, be incubated growing the grain 1.5h, then will material
Liquid is slowly put into centrifugation apparatus, and after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl wet product.Methanol solution
Concentration be 65%；The consumption of methanol solution is 5.5 times of organic phase volume.
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, azo-bis-iso-dimethyl dry product is obtained；It is dry
Dry room temperature≤25 DEG C.
Calculated yield is simultaneously tested to product, and the yield of azo-bis-iso-dimethyl is 93.5% in the present embodiment,
Product purity is 99.80%.
Claims (6)
1. a kind of azo-bis-iso-dimethyl synthetic method, it is characterised in that：It comprises the steps：
（1）Condensation：Azodiisobutyronitrile, methanol, isophorone are added in reaction vessel, the lower addition phosphorus trichloride of stirring is molten
Liquid is reacted, and reaction is finished, and feed liquid is centrifuged, and obtains azoimide methyl ether hydrochloride solid material；
（2）Hydrolysis：Pure water is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride solid material is in stirring
Mix down and be added to hydrolysis vessels and be hydrolyzed；
（3）Split-phase：Feed liquid after hydrolysis is put into split-phase container, divided with consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Phase, split-phase is finished is pressed into crystallisation vessel by upper organic phase；
（4）Recrystallization：Methanol solution addition crystallisation vessel is recrystallized, azo-bis-iso-dimethyl wet product is obtained；
（5）Dry：Wet product is positioned in hothouse and spontaneously dries 24h, room temperature≤25 DEG C are dried.
2. a kind of azo-bis-iso-dimethyl synthetic method according to claim 1, it is characterised in that：Step（1）Contracting
Closing step is：The azodiisobutyronitrile measured, methanol, isophorone are added in reaction vessel, start stirring, three are added dropwise
Insulation reaction 8-15 hours after chlorination phosphorus solution, 10-30 DEG C of reaction temperature, completion of dropping；Feed liquid is centrifuged, azo is obtained
Imines methyl ether hydrochloride solid material；Mass concentration >=95% of the phosphorus trichloride solution；The mol ratio of above-mentioned raw materials is azo two
Isobutyronitrile：Methanol：Isophorone：Phosphorus trichloride=1：2-3.5：3.2-5.8：2-2.8.
3. a kind of azo-bis-iso-dimethyl synthetic method according to claim 1, it is characterised in that：Step（2）Water
Solving step is：The pure water measured is added in hydrolysis vessels, by step（1）Obtained azoimide methyl ether hydrochloride solid material
Hydrolysis vessels are added to stirring, 10-30 DEG C of temperature is controlled, and treat that the addition of azoimide methyl ether hydrochloride is finished, regulation system
PH value is hydrolyzed for 4-9；Azoimide methyl ether hydrochloride solid material and the weight of water ratio 1：2-4.5.
4. a kind of azo-bis-iso-dimethyl synthetic method according to claim 1, it is characterised in that the step（3）
Split-phase step is：Consisting of phase-transferring agent hexadecyltrimethylammonium chloride is added into split-phase container, temperature is maintained at 18-22 DEG C, standing
2-4h carries out split-phase, and split-phase is finished is pressed into crystallisation vessel by upper organic phase；Consisting of phase-transferring agent hexadecyltrimethylammonium chloride
Addition is 0.05-0.5 times of hydrolyzation material volume.
5. a kind of azo-bis-iso-dimethyl synthetic method according to claim 1, it is characterised in that the step（4）
Re-crystallization step is：The methanol solution measured is added in crystallisation vessel, 20-25 DEG C of temperature is controlled, treats that organic phase is complete
Start slow cooling after dissolving, temperature slows down cooling rate when being down to 10 DEG C, it was observed that when having crystal precipitation in crystallisation vessel, putting
Slow mixing speed, accelerates cooling rate after crystal is largely separated out, temperature is down to after 0 DEG C, growing the grain 1-3h is incubated, then by feed liquid
Centrifugation apparatus slowly is put into, after high speed centrifugation after feed liquid separation, discharge to obtain azo-bis-iso-dimethyl wet product.
6. a kind of azo-bis-iso-dimethyl synthetic method according to claim 5, it is characterised in that methanol solution
Concentration is 65%；The consumption of methanol solution is 2.5-5.5 times of organic phase volume.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256281A (en) * | 2018-11-20 | 2019-09-20 | 上海试四赫维化工有限公司 | A kind of preparation method of azo-bis-iso-dimethyl |
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| US3306888A (en) * | 1963-12-09 | 1967-02-28 | Monsanto Co | Azo compounds |
| DE2254572A1 (en) * | 1972-11-08 | 1974-05-22 | Bayer Ag | Azodiisobutyrates prodn. - from azodiisobutyronitrile, alcohol and hydro-chloric acid |
| JPH10101635A (en) * | 1996-09-27 | 1998-04-21 | Wako Pure Chem Ind Ltd | New production of azo ester compound |
| CN104945275A (en) * | 2014-03-28 | 2015-09-30 | 巩龙海 | Method for producing dimethyl 2,2'-azobis(2-methylpropionate) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256281A (en) * | 2018-11-20 | 2019-09-20 | 上海试四赫维化工有限公司 | A kind of preparation method of azo-bis-iso-dimethyl |
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