CN105272947A - Continuous epichlorohydrin production method - Google Patents
Continuous epichlorohydrin production method Download PDFInfo
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- CN105272947A CN105272947A CN201410355477.1A CN201410355477A CN105272947A CN 105272947 A CN105272947 A CN 105272947A CN 201410355477 A CN201410355477 A CN 201410355477A CN 105272947 A CN105272947 A CN 105272947A
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Abstract
The present invention relates to a continuous epichlorohydrin production method. A purpose of the present invention is mainly to solve the problems of low raw material utilization rate and explosion risk caused by the easy peroxide decomposition due to heating in the prior art. According to the present invention, in the presence of a homogeneous molybdenum-based catalyst, an organic peroxide and allyl chloride are used to prepare the epichlorohydrin; the method comprises that: a) a reaction apparatus comprising n reaction kettles connected in series is provided; b) allyl chloride and a catalyst are supplied to the inlet of the first reaction kettle; c) an organic peroxide is divided into n parts, and the n parts are respectively supplied to the inlets of the n reaction kettles; d) except the last reaction kettle, the streams outflowing from the outlets of each reaction kettle enter the inlets of the next reaction kettles, and stream Vn is obtained at the outlet of the last reaction kettle; and e) one part stream Vn' is shunted from the stream Vn, the stream Vn' circulates to the inlet of the first reaction kettle, and the remaining part Vn" is subjected to refining separation so as to obtain the product epichlorohydrin; and the method can be used for the industrial production of the epichlorohydrin.
Description
Technical field
The present invention relates to a kind of method of continuous seepage epoxy chloropropane.
Background technology
Epoxy chloropropane alias table chloropharin, chemical name is chloro-l, the 2-propylene oxide of 3-, is a kind of important Organic Chemicals and synthetic intermediate.In epoxy compounds, the output of epoxy chloropropane is only second to oxyethane and propylene oxide, occupies the 3rd.Epoxy chloropropane can be used as the solvent of cellulose ester, resin and ether of cellulose, is also the raw material producing tensio-active agent, medicine, agricultural chemicals, coating, sizing agent, ion exchange resin, softening agent, glycerol derivative and glycidyl derivatives.Each based epoxy resin prepared by epoxy chloropropane and dihydroxyphenyl propane has the features such as tackiness is strong, shrinkability is little, resistance to chemical attack, good stability, is widely used as coating, tamanori, strongthener and cast material etc.The new variety of to take epoxy chloropropane as the chlorohydrin rubber of raw material production be rubber, not easily expand, have the peculiar function of larger flexibility (being better than butyronitrile, chloroprene rubber and isoprene-isobutylene rubber) under low temperature exists without softening agent in usual vehicle.As a kind of important Organic Chemicals and fine chemical product, epoxy chloropropane is widely used in the industries such as chemical industry, light industry, medicine, electronic apparatus.
Current epoxy chloropropane production method mainly contains 3 kinds: take propylene as the propylene high-temperature chlorination process of raw material, acetate propylene ester process and take glycerine as the glycerine method of raw material.Propylene high-temperature chlorination process was applied to suitability for industrialized production in 1948 by U.S.'s Shell company First Successful Development, was the classical way producing epoxy chloropropane.At present, the epoxy chloropropane of more than 90% adopts the method to produce in the world.But the shortcoming of this technique is raw material chlorine severe corrosion equipment, require high to the material of purified propylene and reactor, energy consumption is large, chlorine consumption is large, and by product is many, product yield low (about 70%), the chloride containing calcium produced in production, the sewage quantity of organic chloride are large, processing costs is high, and easy coking, coke cleaning period is short.For this shortcoming, people develop the epoxy chloropropane preparation method made new advances.Document CN201010522944.7 discloses a kind of propenyl chloride Direct Epoxidation epoxy chloropropane method, the method is under the existence of additive phosphoric acid quaternary ammonium salt, the excessive propenyl chloride of relative Oxidation agent, under the effect of catalyzer quaternary ammonium salt phosphor-tungstic heteropoly acid, is that oxygenant reacts at reflux and directly generates epoxy chloropropane with hydrogen peroxide.This catalyzer is dissolved in reaction solution when reacting, and reaction terminates rear precipitation, but there is the problem that catalyzer can not dissolve completely and can not separate out completely, directly can have influence on activity and the rate of recovery of catalyzer like this.Document CN101747297A discloses a kind of method of continuous seepage epoxy chloropropane, the method comprises introduces multiple fixed-bed reactor that titanium-silicon molecular sieve catalyst is housed by chlorallylene, hydrogen peroxide and solvent, makes chlorallylene and hydrogen peroxide carry out epoxidation reaction; In at least one fixed-bed reactor, stop epoxidation reaction, by catalyst regeneration wherein, wherein, any one reactor, when carrying out the regeneration of catalyzer, has epoxidation reaction to carry out at least one reactor in other reactor.But the method adopts hydrogen peroxide as oxygenant, because pyrolytic decomposition met by hydrogen peroxide, the utilization ratio of raw material can decline on the one hand, and peroxide decomposition can produce oxygen on the other hand, and oxygen and propenyl chloride are mixed with explosion hazard.
Summary of the invention
Technical problem to be solved by this invention is that prior art exists superoxide and is heated and easily decomposes, and causes the problem that raw material availability is low, have explosion hazard, provides a kind of method of new continuous seepage epoxy chloropropane.It is high that the method has raw material availability, and temperature is easy to control, remove the fast feature of heat.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method of continuous seepage epoxy chloropropane, under the existence of homogeneous phase catalyst with base of molybdenum, prepares epoxy chloropropane by organo-peroxide and propenyl chloride; The method comprises the following steps:
A) reaction unit comprising n cascade reaction still is provided; Wherein, n is the integer of more than 2;
B) containing the material flow A of fresh propenyl chloride with supply first reactor entrance containing the flow C of homogeneous phase catalyst with base of molybdenum;
C) flow B containing organo-peroxide is divided into n part, supplies n reactor entrance respectively;
D) except last reactor, the logistics flowed out from the outlet of each reactor enters next reactor entrance, thus in the end a reactor outlet obtains logistics V
n;
E) described logistics V
ndistribute a part of V
n', V
n' be circulated to first reactor entrance; Remainder V
n" after refining spearation, obtain product epoxy chloropropane;
Wherein, the temperature of reaction controlling each reactor is 30 ~ 200 DEG C, and T
n>=T
n-1, make except last reactor, in each reactor, the transformation efficiency of superoxide is all less than 100%, and in last reactor, the transformation efficiency of superoxide is 100%.
In technique scheme, preferably, logistics V
n' account for logistics V
nweight percent be 10 ~ 60%.More preferably, logistics V
n' account for logistics V
nweight percent be 30 ~ 50%.
In technique scheme, preferably, the consumption of described homogeneous phase catalyst with base of molybdenum is counted with molybdenum: in molybdenum and flow B, the weight ratio of organo-peroxide is 0.00001 ~ 0.0005.More preferably, in molybdenum and flow B, the weight ratio of organo-peroxide is 0.00005 ~ 0.0004.
In technique scheme, preferably, in material flow A, in propenyl chloride and flow B, the mol ratio of organo-peroxide is 1 ~ 10, is more preferably 3 ~ 8.
In technique scheme, preferably, the temperature of reaction of each reactor is 40 ~ 150 DEG C.
In technique scheme, preferably, reaction pressure is 0.01 ~ 2.0MPa, is more preferably 0.1 ~ 1.5MPa.
In technique scheme, preferably, n is the integer of 2 ~ 6.
In technique scheme, preferably, except last reactor, in each reactor, the transformation efficiency of superoxide is 0 ~ 70%, but is not 0.
In technique scheme, preferably, described organo-peroxide is selected from the cumene solution of hydrogen phosphide cumene or the ethylbenzene solution of hydrogen peroxide ethylbenzene.
In technique scheme, preferably, the flow B containing organo-peroxide is divided into n part, supplies n reactor entrance respectively.
The preparation method of the homogeneous phase catalyst with base of molybdenum described in the inventive method is as follows:
A) molybdenum source and acidic substance are dissolved in solvent, obtain mixture I; Wherein said molybdenum source is selected from least one in molybdenum oxide, molybdic acid, acetyl acetone or Ammonium Heptamolybdate, described acidic substance are selected from least one in isocaprylic acid, naphthenic acid, NSC 60134, caproic acid or hydrochloric acid, sulfuric acid or nitric acid, described solvent is selected from ethylbenzene, α, at least one in alpha-alpha-dimethyl benzylalcohol, xylyl alcohol or isopropyl benzene, the weight ratio of molybdenum source and acid solvent is 1:(5 ~ 20), the weight ratio of molybdenum source and solvent is 1:(2 ~ 10).
B) in mixture I, add organic amine, be heated to 120 ~ 200 DEG C, stir 1 ~ 24 hour, obtain mixture II; Wherein, described organic amine is selected from molecular formula is C
nh
2nnH
3chain alkyl amine, n=6 ~ 18, or at least one in pyridine compounds and their, the consumption of organic amine is 1:(1 ~ 10 of molybdenum source weight).
C) in mixture II, add alkaline matter, stirring at room temperature 0.5 ~ 12 hour, namely obtain described homogeneous phase molybdenum basic ring oxide catalyst; Wherein, described alkaline matter is selected from least one in sodium napthionate, sodium carbonate or carbonyl magnesium, sodium bicarbonate, sodium-acetate, and the consumption of alkaline matter is 1:(10 ~ 50 of molybdenum source weight).
Wherein, at least one in the preferred cetylamine of chain alkyl amine or stearylamine, at least one in the preferred 2-amino of pyridine compounds and their-6-picoline, o-aminopyridine, 2-bromopyridine or 2 hydroxy pyrimidine.
Adopt the inventive method, the logistics V containing epoxy chloropropane that an in the end reactor outlet obtains
n, a part of V
n' loop back first reactor entrance, remainder V
n" after refining spearation, epichlorohydrin product can be obtained.Take organo-peroxide as the ethylbenzene solution of hydrogen peroxide ethylbenzene be example, the process of separation can comprise the following steps:
1) logistics V
n" enter distillation tower I, after separation, obtain the first heavy constituent logistics containing ethylbenzene, epoxy chloropropane and methylbenzyl alcohol at the bottom of tower, tower top obtains the first light component stream containing unreacted propenyl chloride; Described first light component stream can be circulated to first reactor ingress, together enters reactor react with fresh propenyl chloride material flow A;
2) described first heavy constituent logistics enters distillation tower II, and after separation, obtain the second heavy constituent logistics containing epoxy chloropropane and methylbenzyl alcohol at the bottom of tower, tower top obtains the second light component stream containing ethylbenzene; Described second light component stream can be circulated to first reactor ingress, together enters reactor react with the flow B containing superoxide;
3) described second heavy constituent logistics enters distillation tower III, and after separation, obtain the triple component streams containing methylbenzyl alcohol at the bottom of tower, the 3rd light component stream that tower top obtains is epoxy chloropropane product stream.
Wherein, the operational condition of distillation tower I is: stage number is 2 ~ 70 pieces, and pressure is 0.01 ~ 3MPa, and tower top temperature is 0 ~ 80 DEG C, and column bottom temperature is 0 ~ 200 DEG C.Preferable range is: stage number is 2 ~ 50 pieces, and pressure is 0.01 ~ 2MPa, and tower top temperature is 0 ~ 60 DEG C, and column bottom temperature is 0 ~ 150 DEG C.
The operational condition of distillation tower II is: stage number is 2 ~ 70 pieces, and pressure is 0.01 ~ 3MPa, and tower top temperature is 0 ~ 120 DEG C, and column bottom temperature is 0 ~ 300 DEG C.Preferable range is: stage number is 2 ~ 50 pieces, and pressure is 0.01 ~ 2MPa, and tower top temperature is 0 ~ 100 DEG C, and column bottom temperature is 0 ~ 250 DEG C.
The operational condition of distillation tower III is: stage number is 2 ~ 70 pieces, and pressure is 0.01 ~ 5MPa, and tower top temperature is 0 ~ 150 DEG C, and column bottom temperature is 0 ~ 400 DEG C.Preferable range is: stage number is 2 ~ 50 pieces, and pressure is 0.01 ~ 4MPa, and tower top temperature is 0 ~ 130 DEG C, and column bottom temperature is 0 ~ 350 DEG C.
Transformation efficiency described in the inventive method refers to the transformation efficiency of organo-peroxide, and the transformation efficiency of each reactor is the concentration based on the organo-peroxide in feed stream B.
The present invention produces epoxy chloropropane by propenyl chloride and organo-peroxide, adopt the mode of continuously feeding, reactor adopts n reactor series connection to use, propenyl chloride enters from first reactor top, organo-peroxide is divided into n part, supply n reactor entrance respectively, except last reactor, the logistics that outlet flow goes out bottom each reactor enters next reactor top entry respectively, the logistics that the outlet of last reactor is flowed out distributes a part and is circulated to first reactor entrance, the temperature of reaction of a rear reactor is greater than or equal to previous reactor, from last reactor material out, the content of superoxide is zero.By regulating the temperature of reaction of each reactor, regulating and controlling the transformation efficiency of reactant, to reach control exothermic heat of reaction, preventing the danger that peroxide breakdown is brought.So both can prevent the runaway reaction with heating, what can ensure again to react carries out continuously, and therefore the method has temperature and is easy to control, remove the fast feature of heat, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 is the inventive method process flow diagram.
In Fig. 1,1 ~ n is reactor, and material flow A is fresh propenyl chloride, and flow B is the logistics containing organo-peroxide, and flow C is the homogeneous phase catalyst with base of molybdenum logistics containing 1.5 % by weight molybdenums, V
1, V
2vn is from first, second ... the logistics that n-th reactor outlet is flowed out, Vn ' is the logistics distributing, loop back first reactor from Vn, V
n" be the product stream containing epoxy chloropropane.
In Fig. 1, material flow A and catalyzer C enter from the top of first reactor, and flow B is divided into n part, supply n reactor entrance respectively, and enter from each reactor top.Except last reactor, the logistics that outlet flow goes out bottom each reactor enters next reactor top entry respectively, and the logistics Vn flowed out from the outlet of last reactor distributes a part of Vn ', is circulated to first reactor entrance, remainder V
n" after refining spearation, epichlorohydrin product can be obtained.
Below by embodiment, the invention will be further elaborated.
Embodiment
Prepare homogeneous phase catalyst with base of molybdenum:
Get 1.2 grams of commercial grade molybdenum oxides, add 30 grams of naphthenic acid and 20 grams of isopropyl benzenes, stirring at room temperature 1 day, molybdenum compound progressively dissolves, and mixture color progressively changes brown into by glassy yellow; Then add 0.24 gram of cetylamine, be heated to 170 DEG C, magnetic agitation 12 hours; Then add sodium napthionate 0.2 gram, stir 0.5 hour, obtain homogeneous phase organic-molybdenum catalyzer.Wherein, in molybdenum, in catalyzer, molybdenum content is 1.5 % by weight.
[embodiment 1]
Adopt flow process shown in Fig. 1,2 reactors series connection use, and flow is that the homogeneous phase catalyst with base of molybdenum that fresh propenyl chloride and the flow of 1.7 kgs/hr is 3.3 Grams Per Hours mixes, and enters from reactor 1 top.From reaction 2 still discharging V2 ', distributing 30% with flow is, after 2 kgs/hr of ethylbenzene solutions containing 50% ethylbenzene hydroperoxide mix, be divided into 2 equal portions, enter respectively from the top entry of reactor 1 and reactor 2.
The weight ratio of molybdenum and ethylbenzene hydroperoxide is 0.00005, epoxy chloropropane: ethylbenzene hydroperoxide=3 (mol ratio).
The temperature of reaction of reactor 1 30 DEG C, reaction pressure 0.1MPa, the transformation efficiency of ethylbenzene hydroperoxide is 50%.
The temperature of reaction of reactor 2 50 DEG C, reaction pressure 0.1MPa, the transformation efficiency of ethylbenzene hydroperoxide is 100%.
Result: epoxy chloropropane is 98% to the selectivity of ethylbenzene hydroperoxide, the transformation efficiency of ethylbenzene hydroperoxide is 100%, the yield 98% of epoxy chloropropane.
[embodiment 2]
Adopt flow process shown in Fig. 1,4 reactors series connection use, and flow is that the homogeneous phase catalyst with base of molybdenum that fresh propenyl chloride and the flow of 2.5 kgs/hr is 6.7 Grams Per Hours mixes, and enters reactor from reactor 1 top.From last reactor discharging V
4' in distribute 40% with flow be, after 2 kgs/hr of cumene solutions containing 50% isopropyl benzene hydroperoxide mix, be divided into 4 equal portions, enter respectively from reactor 1 to the top entry of reactor 4.
The weight ratio of molybdenum and isopropyl benzene hydroperoxide is 0.0001, propenyl chloride: isopropyl benzene hydroperoxide=5 (mol ratio).
The temperature of reaction of reactor 1 30 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 30%.
The temperature of reaction of reactor 2 40 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 60%.
The temperature of reaction of reactor 3 50 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 90%.
The temperature of reaction of reactor 4 60 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 100%.
Result: epoxy chloropropane is 99% to the selectivity of isopropyl benzene hydroperoxide, the transformation efficiency of isopropyl benzene hydroperoxide is 100%, the yield 99% of epoxy chloropropane.
[embodiment 3]
Adopt flow process shown in Fig. 1,5 reactors series connection use, and flow is that the homogeneous phase catalyst with base of molybdenum that fresh propenyl chloride and the flow of 3.92 kgs/hr is 20 Grams Per Hours mixes, and enters from reactor 1 top.From last reactor discharging V
5' in distribute 50% with flow be, after 2 kgs/hr of ethylbenzene solutions containing 50% ethylbenzene hydroperoxide mix, be divided into 5 equal portions, enter respectively from reactor 1 to the top entry of reactor 5.
The weight ratio of molybdenum and ethylbenzene hydroperoxide is 0.0003, propenyl chloride: ethylbenzene hydroperoxide=7 (mol ratio).
The temperature of reaction of reactor 1 30 DEG C, reaction pressure 0.7MPa, the transformation efficiency of ethylbenzene hydroperoxide is 35%.
The temperature of reaction of reactor 2 50 DEG C, reaction pressure 0.7MPa, the transformation efficiency of ethylbenzene hydroperoxide is 55%.
The temperature of reaction of reactor 3 90 DEG C, reaction pressure 0.7MPa, the transformation efficiency of ethylbenzene hydroperoxide is 75%.
The temperature of reaction of reactor 4 100 DEG C, reaction pressure 0.7MPa, the transformation efficiency of ethylbenzene hydroperoxide is 95%.
The temperature of reaction of reactor 5 110 DEG C, reaction pressure 0.7MPa, the transformation efficiency of ethylbenzene hydroperoxide is 100%.
Result: epoxy chloropropane is 99% to the selectivity of ethylbenzene hydroperoxide, the transformation efficiency of ethylbenzene hydroperoxide is 100%, the yield 99% of epoxy chloropropane.
[embodiment 4]
Adopt flow process shown in Fig. 1,6 reactors series connection use, and flow is that the homogeneous phase catalyst with base of molybdenum that fresh propenyl chloride and the flow of 4 kgs/hr is 26.7 Grams Per Hours mixes, and enters reactor from reactor 1 top.From last reactor discharging V
6' in distribute 35% with flow be, after 2 kgs/hr of cumene solutions containing 50% isopropyl benzene hydroperoxide mix, be divided into 6 equal portions, enter respectively from reactor 1 to the top entry of reactor 6.
The weight ratio of molybdenum and isopropyl benzene hydroperoxide is 0.0004, propenyl chloride: isopropyl benzene hydroperoxide=8 (mol ratio).
The temperature of reaction of reactor 1 60 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 40%.
The temperature of reaction of reactor 2 80 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 55%.
The temperature of reaction of reactor 3 90 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 60%.
The temperature of reaction of reactor 4 100 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 80%.
The temperature of reaction of reactor 5 110 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 95%.
The temperature of reaction of reactor 6 120 DEG C, reaction pressure 1MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 100%.
Result: epoxy chloropropane is 99% to the selectivity of isopropyl benzene hydroperoxide, the transformation efficiency of isopropyl benzene hydroperoxide is 100%, the yield 99% of epoxy chloropropane.
[comparative example 1]
Adopt 1 reactor to carry out chloro propylene epoxidation reaction, the homogeneous phase catalyst with base of molybdenum that flow is the fresh propenyl chloride of 0.5 kg/hr is 26.7 Grams Per Hours with the circulation propenyl chloride of 3.5 kgs/hr and flow mixes, and enters from reactor top.Flow is, after 2 kgs/hr of cumene solutions containing 50% isopropyl benzene hydroperoxide mix with 1 kg/hr of circulation isopropyl benzene, enter from the top entry of reactor.
The weight ratio of molybdenum and isopropyl benzene hydroperoxide is 0.0004, propenyl chloride: isopropyl benzene hydroperoxide=8 (mol ratio).
The temperature of reaction of reactor 80 DEG C, reaction pressure 0.5MPa.
The flow of the epoxy chloropropane product obtained is 0.34 kg/hr, and epoxy chloropropane is 65% to the selectivity of isopropyl benzene hydroperoxide, and the transformation efficiency of isopropyl benzene hydroperoxide is 85%, the yield 55% of epoxy chloropropane.
[comparative example 2]
Adopt flow process shown in Fig. 1,4 reactor series connection use, just V
4in do not have by-passing portions to be circulated to reactor 1.Flow is that the homogeneous phase catalyst with base of molybdenum that fresh propenyl chloride and the flow of 2.5 kgs/hr is 6.7 Grams Per Hours mixes, and enters reactor from reactor 1 top.Flow is, after 2 kgs/hr of cumene solutions containing 50% isopropyl benzene hydroperoxide mix with 1 kg/hr of circulation isopropyl benzene, be divided into 4 equal portions, enter respectively from reactor 1 to the top entry of reactor 4.
The weight ratio of molybdenum and isopropyl benzene hydroperoxide is 0.0001, propenyl chloride: isopropyl benzene hydroperoxide=5 (mol ratio).
The temperature of reaction of reactor 1 60 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 60%.
The temperature of reaction of reactor 2 50 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 65%.
The temperature of reaction of reactor 3 40 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 68%.
The temperature of reaction of reactor 4 30 DEG C, reaction pressure 0.3MPa, the transformation efficiency of isopropyl benzene hydroperoxide is 69%.
Result: epoxy chloropropane is 95% to the selectivity of isopropyl benzene hydroperoxide, the transformation efficiency of isopropyl benzene hydroperoxide is 69%, the yield 65% of epoxy chloropropane.
Claims (10)
1. a method for continuous seepage epoxy chloropropane, under the existence of homogeneous phase catalyst with base of molybdenum, prepares epoxy chloropropane by organo-peroxide and propenyl chloride; The method comprises the following steps:
A) reaction unit comprising n cascade reaction still is provided; Wherein, n is the integer of more than 2;
B) containing the material flow A of fresh propenyl chloride with supply first reactor entrance containing the flow C of homogeneous phase catalyst with base of molybdenum;
C) flow B containing organo-peroxide is divided into n part, supplies n reactor entrance respectively;
D) except last reactor, the logistics flowed out from the outlet of each reactor enters next reactor entrance, thus in the end a reactor outlet obtains logistics V
n;
E) described logistics V
ndistribute a part of V
n', V
n' be circulated to first reactor entrance; Remainder V
n" after refining spearation, obtain product epoxy chloropropane;
Wherein, the temperature of reaction controlling each reactor is 30 ~ 200 DEG C, and T
n>=T
n-1, make except last reactor, in each reactor, the transformation efficiency of superoxide is all less than 100%, and in last reactor, the transformation efficiency of superoxide is 100%.
2. the method for continuous seepage epoxy chloropropane according to claim 1, is characterized in that logistics V
n' account for logistics V
nweight percent be 10 ~ 60%.
3. the method for continuous seepage epoxy chloropropane according to claim 2, is characterized in that logistics V
n' account for logistics V
nweight percent be 30 ~ 50%.
4. the method for continuous seepage epoxy chloropropane according to claim 1, is characterized in that the consumption of described homogeneous phase catalyst with base of molybdenum is counted with molybdenum: in molybdenum and flow B, the weight ratio of organo-peroxide is 0.00001 ~ 0.0005; In material flow A, in propenyl chloride and flow B, the mol ratio of organo-peroxide is 1 ~ 10.
5. the method for continuous seepage epoxy chloropropane according to claim 4, is characterized in that the consumption of described homogeneous phase catalyst with base of molybdenum is counted with molybdenum: in molybdenum and flow B, the weight ratio of organo-peroxide is 0.00005 ~ 0.0004; In material flow A, in propenyl chloride and flow B, the mol ratio of organo-peroxide is 3 ~ 8.
6. the method for continuous seepage epoxy chloropropane according to claim 1, it is characterized in that the temperature of reaction of each reactor is 40 ~ 150 DEG C, reaction pressure is 0.01 ~ 2.0MPa.
7. the method for continuous seepage epoxy chloropropane according to claim 6, is characterized in that the reaction pressure of each reactor is 0.1 ~ 1.5MPa.
8. the method for continuous seepage epoxy chloropropane according to claim 1, is characterized in that n is the integer of 2 ~ 6.
9. the method for continuous seepage epoxy chloropropane according to claim 1, it is characterized in that except last reactor, in each reactor, the transformation efficiency of superoxide is 0 ~ 70%, but is not 0.
10. the method for continuous seepage epoxy chloropropane according to claim 1, is characterized in that described organo-peroxide is selected from the cumene solution of hydrogen phosphide cumene or the ethylbenzene solution of hydrogen peroxide ethylbenzene.
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| CN112250643A (en) * | 2020-10-26 | 2021-01-22 | 北京水木滨华科技有限公司 | Preparation method of epoxy compound |
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| CN101279958A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane by epoxidation of propylene chloride |
| CN101885711A (en) * | 2009-05-13 | 2010-11-17 | 中国石油化工股份有限公司 | Production method of propylene oxide |
| CN103539762A (en) * | 2012-07-12 | 2014-01-29 | 中国石油化工股份有限公司 | Method for producing epoxypropane by propylene epoxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279958A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane by epoxidation of propylene chloride |
| CN101885711A (en) * | 2009-05-13 | 2010-11-17 | 中国石油化工股份有限公司 | Production method of propylene oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250643A (en) * | 2020-10-26 | 2021-01-22 | 北京水木滨华科技有限公司 | Preparation method of epoxy compound |
| CN112250643B (en) * | 2020-10-26 | 2022-02-11 | 北京水木滨华科技有限公司 | Preparation method of epoxy compound |
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