CN206318907U - A kind of device for preparing expoxy propane - Google Patents

A kind of device for preparing expoxy propane Download PDF

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CN206318907U
CN206318907U CN201621445741.1U CN201621445741U CN206318907U CN 206318907 U CN206318907 U CN 206318907U CN 201621445741 U CN201621445741 U CN 201621445741U CN 206318907 U CN206318907 U CN 206318907U
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bed reactor
paste state
state bed
propylene
tank diameter
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刘国东
李进
王炳春
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Dalian Heterogeneous Catalyst Co Ltd
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Dalian Heterogeneous Catalyst Co Ltd
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The utility model discloses a kind of device for preparing expoxy propane.Described device, include bubble tower paste state bed reactor, sedimentation separation unit, tank diameter paste state bed reactor successively, in 0.1~0.6MPa of reaction pressure, under the reaction condition that 40~70 DEG C of reaction temperature, the method for carrying out epoxidation reaction using the combination of bubble tower paste state bed reactor and tank diameter paste state bed reactor.Strongly exothermic generation hot localised points in course of reaction can be prevented effectively from, liquid phase back mixing generation accessory substance can be also prevented effectively from.It is high (>=99%) with hydrogen peroxide conversion, the advantage of effective utilization ratio of hydrogen peroxide good (>=95%) and product propene oxide selectivity high (>=98%).

Description

A kind of device for preparing expoxy propane
Technical field
The utility model is related to the device that a kind of alkene epoxidation prepares expoxy propane.
Background technology
Expoxy propane is to be only second to polypropylene and the fine the third-largest acryloyl derivative of propylene, is very important to have substantially Machine industrial chemicals, it manufactures polyurethane mainly for the production of PPG.Expoxy propane can also be used to produce nonionic Surfactant and propenyl, propane diols, synthetic glycerine etc..Fine chemicals derived from expoxy propane is almost applied to all works In industry department and daily life.
Chlorohydrination, conjugated oxidation and direct oxidation method are the Producing Process of Propylene Oxide of industrial relative maturity at present.It is special Not, it is catalyst using HTS, uses method (the abbreviation HPPO of hydrogen peroxide direct oxidation synthesizing epoxypropane Method), it is serious to equipment corrosion to overcome chlorohydrination, the inferior position such as waste liquid, waste residue are more;Also conjugated oxidation production co-product is not present many Deficiency, be internationally recognized environment-friendly production technology.Therefore, HPPO techniques will turn into newly-built within one period from now on The main production that expoxy propane project is used.
The method that substantial amounts of patent discloses preparing epoxypropane by epoxidation of propene, for example:
The organic compound and hydroperoxidation that the double bond containing C=C is disclosed in WO2000/007965 prepare epoxy compound The method of thing, reaction is carried out in two steps altogether, and first step reaction is carried out in isothermal fixed bed, and second step is reacted insulation fix bed Middle to carry out, reaction pressure is self-generated pressure~100Bar.
Disclosed in WO2004/013116 and carry out epoxidised technique using two fixed beds, the first step is reacted in isothermal Carried out in fixed bed, second step reaction is that fixed bed there are multiple feedstocks the characteristics of insulation fix bed middle progress, this method Point and product exit point.
CN102442976A discloses a kind of olefin epoxidation process, and this method comprises the following steps:(1) in olefin epoxide Change under conditions of reaction, under the existence condition of the first solid catalyst, make first containing solvent, alkene and hydrogen peroxide to mix Compound material carries out epoxidation reaction in moving-burden bed reactor, the degree of reaction make the conversion ratio of hydrogen peroxide reach 50% with On;(2) reactant mixture for obtaining step (1) under the reaction condition of alkene epoxidation and the second solid catalyst are introduced Epoxidation reaction is carried out into slurry bed reactor, the degree of reaction makes the total conversion of hydrogen peroxide reach more than 95%.Institute The reaction pressure for stating moving-burden bed reactor and slurry bed reactor is 0.5~4.5MPa, preferably 0.6~3MPa.This utility model Hydrogen peroxide conversion low shortcoming when only being reacted using moving bed is overcome, is only entered while also overcoming using slurry bed Have the shortcomings that expoxy propane is selectively low during row reaction, wherein the slurry-bed reaction is intermittent reaction.
CN104311513A discloses a kind of method for preparing expoxy propane, this method using fixed bed pipeline reactor and The technique of slurry reactor kettle combination.The method includes the steps of:(1) reaction raw materials propylene, peroxide are added into reactor Change hydrogen, solvent methanol and titanium silicalite catalyst and set up circulation;(2) reaction raw materials and solvent are continuously added to pipe outside reactor Road reactor is reacted, then feeding reactor is reacted after being mixed through static mixer.Hydrogen peroxide in this utility model Conversion ratio >=96%, selectivity >=95% of expoxy propane is reacted for successive reaction, reacting balance.
CN104557781A discloses a kind of method for producing expoxy propane, mainly solves prior art and there is reaction temperature rising It is higher, and be the mol ratio problem of the higher propylene of the higher reaction efficiency needs of holding and peroxide.This utility model Enter at least two sections of multistage insulation reaction zone using raw material propylene and cumyl hydroperoxide, wherein reaction pressure 1.0~ 12.0MPa;The segmentation of raw material hydrogen peroxide isopropylbenzene enters each beds of multistage insulation reaction zone;Multistage insulation reaction zone Export each beds entrance that the obtained epoxidation product containing expoxy propane is partly recycled to multistage insulation reaction zone, mesh The selectivity of mark product propene oxide reaches 96.4%.
It is due to epoxidation although HPPO techniques have process environment friendly and the coproduction accessory substance remarkable advantage such as less There is substantial amounts of solvent (such as methanol), water and excessive propylene in course of reaction, and epoxidation reaction of olefines is strongly exothermic Reaction, therefore, HPPO techniques still suffer from low production efficiency, and raw material (hydrogen peroxide) conversion is incomplete, and reacting strongly exothermic may lead Cause temperature runaway so as to reaction unit and catalyst are caused damage wait deficiency.
Above-mentioned each publication, for preparing epoxypropane by epoxidation of propene method, employs fixed bed, moving bed, slurry The technique such as state bed and moving bed and slurry bed system combination, targetedly solves epoxidization reaction process heat release, raw material respectively The problems such as under conversion ratio deficiency and low production efficiency.But from the point of view of the report of existing literature and patent, it is still desirable to which exploitation is new Epoxidation of propylene technique so that simply and efficiently solve HPPO technical process present in hydrogen peroxide conversion not exclusively, mistake Hydrogen oxide effective rate of utilization is not high, product propene oxide is selectively low, react strongly exothermic may cause the problems such as temperature runaway.
Utility model content
Technical problem to be solved in the utility model is for being deposited in existing HPPO methods production propylene oxide process technology Deficiency, and provide a kind of device for preparing expoxy propane.
To achieve these goals, the utility model is adopted the following technical scheme that:
A kind of device for preparing expoxy propane, successively including bubble tower paste state bed reactor, sedimentation separation unit, tank diameter Paste state bed reactor, bubble tower paste state bed reactor bottom adds mouth provided with methanol/hydrogen peroxide and propylene adds mouth B, top Mouth C and propylene outlet E are added provided with catalyst, the propylene outlet E connection tank diameter paste state bed reactors bottom propylene is added Mouth K;The suspension slurry of bubble tower paste state bed reactor middle and upper part is by outlet connection sedimentation separation unit;Sedimentation separation unit bottom Concentrated slurry outlet bubble tower paste state bed reactor bottom;Purified liquor outlet connection tank diameter slurry in the middle part of sedimentation separation unit State bed reactor bottom clear liquid adds mouth H;L is exported provided with propylene and catalyst adds mouth I at the top of tank diameter paste state bed reactor.
Preferably, also including tank diameter paste state bed reactor II, the propylene outlet E, propylene add mouth K, tank diameter slurry The bottom propylene of state bed reactor II adds mouth and is interconnected;Purified liquor outlet, clear liquid add mouth H, tank diameter paste state bed reactor II Bottom clear liquid adds mouth and is interconnected;The top of tank diameter paste state bed reactor II adds mouth provided with propylene outlet and catalyst.
Preferably, metal film separator-filter J is provided with inside tank diameter paste state bed reactor.
Preferably, the inside of tank diameter paste state bed reactor II is provided with metal film separator-filter.
A kind of method that expoxy propane is prepared under lower pressure, be one kind under the conditions of low pressure reaction (0.1~ 0.6MPa), the method for carrying out epoxidation reaction using the combination of bubble tower paste state bed reactor and tank diameter paste state bed reactor. This method can not only be prevented effectively from it is strongly exothermic in course of reaction caused by reactor temperature runaway, and with epoxidation of propylene mistake The conversion ratio of raw material hydrogen peroxide and effective rate of utilization height and the high remarkable advantage of selectivity of propylene oxide in products in journey.
Specifically include following steps:
(1) in bubble tower paste state bed reactor, using methanol as reaction dissolvent, HTS is catalyst, anti- Answer under 0.1~0.6MPa of pressure, the reaction condition that 30~90 DEG C of reaction temperature, propylene and hydrogen peroxide carry out epoxidation reaction.
(2) reacted suspension slurry enters sedimentation separation unit in bubble tower paste state bed reactor, through sedimentation separation Obtain supernatant liquor (mainly comprising expoxy propane, methanol and hydrogen peroxide) and the concentrated slurry containing catalyst.Supernatant liquor enters To enter continue in the tank diameter paste state bed reactor of later procedure and react, and the concentrated slurry containing catalyst then returns to bubble tower slurry Reaction is participated in again in bed reactor.Unreacted gas-phase propene enters stirring for later procedure in bubble tower paste state bed reactor Mix in groove paste state bed reactor and continue to participate in epoxidation reaction.After being reacted through bubble tower paste state bed reactor, raw material hydrogen peroxide Conversion ratio reach more than 80%.
(3) under the catalytic action of Ti-Si zeolite molecular sieve catalyst, the propylene come from bubble tower paste state bed reactor With the clear liquid (mainly comprising expoxy propane, methanol and hydrogen peroxide) come from sedimentation separative element in tank diameter slurry reactor Proceed epoxidation reaction, wherein 0.1~0.6MPa of reaction pressure, 30~90 DEG C of reaction temperature in device.Agitated groove slurry After bed reactor reaction, conversion ratio >=99% of raw material hydrogen peroxide.
(4) reacted liquid product is filtered by metal film filter in tank diameter paste state bed reactor, mistake The clear liquid (mainly comprising methanol and expoxy propane) filtered out enters later separation process, and is stayed in by the catalyst that metal film is retained Reaction is continued to participate in reactor.Reacted gas-phase product (mainly comprising propylene) is also entered in tank diameter paste state bed reactor Enter follow-up separation process.Propylene and methanol loop after being separated through separation circuit are utilized.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, raw material propylene, hydrogen peroxide It is pumped into proportion in reactor with methanol.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, solvent methanol, propylene and mistake The content of hydrogen oxide can change in very large range, under preferable case, the raw material propylene, hydrogen peroxide and solvent methanol Mol ratio is (1.5~5):1:(2~6).
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, 30~90 DEG C of reaction temperature, It is preferred that 40~60 DEG C.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, reaction pressure 0.1~ 0.6MPa, preferably 0.3~0.6MPa.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, divides through sedimentation separation unit From the rear concentrated slurry containing catalyst bubble tower paste state bed reactor is recycled back to using slush pump.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, gas phase and liquid (Gu) mutually may be used Can also forward flow operation, preferably forward flow operation with adverse current.
In above-mentioned technical proposal, described bubble tower paste state bed reactor during the course of the reaction, raw material hydrogen peroxide turn Rate >=80%.
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, divides through sedimentation separation unit Liquid phase clear liquid from after is pumped into tank diameter paste state bed reactor through pump.
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, 30~90 DEG C of reaction temperature, It is preferred that 40~60 DEG C.
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, reaction pressure 0.1~ 0.6MPa, preferably 0.3~0.6MPa.
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, the reaction time 5~ 120min, preferably 60~90min.
In above-mentioned technical proposal, described tank diameter paste state bed reactor totally 2, alternation response, discharge opeing;
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, solvent methanol, propylene and mistake The content of hydrogen oxide can change in very large range, under preferable case, the raw material propylene, hydrogen peroxide and solvent methanol Mol ratio is (1.5~5):1:(2~6).
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, by metal film filter The clear liquid (mainly comprising methanol and expoxy propane) filtered out controls discharge rate with pump, with reference to raw material, solvent and catalyst Constantly add, so as to realize being carried out continuously for expoxy propane preparation technology.
In above-mentioned technical proposal, described tank diameter paste state bed reactor during the course of the reaction, raw material hydrogen peroxide turn Rate reaches more than 99%.
In above-mentioned epoxidation technical scheme, the combination through bubble tower paste state bed reactor and tank diameter paste state bed reactor is anti- Ying Hou, conversion ratio >=99% of raw material hydrogen peroxide, effective rate of utilization >=95% of raw material hydrogen peroxide, product propene oxide Selectivity >=98%.
In above-mentioned technical proposal, the choosing of described hydrogen peroxide conversion, effective utilization ratio of hydrogen peroxide and expoxy propane The computational methods of selecting property are as follows:
In bubble tower paste state bed reactor peroxide is converted in the conversion ratio of hydrogen peroxide=bubble tower paste state bed reactor Change total mole number × 100% of the hydrogen peroxide of molal quantity/charging of hydrogen;
It was converted in the total conversion of hydrogen peroxide=bubble tower paste state bed reactor and tank diameter paste state bed reactor Total mole number × 100% of the hydrogen peroxide of molal quantity sum/charging of hydrogen oxide;
The effective rate of utilization of hydrogen peroxide=(generation expoxy propane molal quantity+generation propane diols molal quantity+generation monomethyl ether Molal quantity)/it is converted total mole number × 100% of hydrogen peroxide;
The molal quantity of expoxy propane selectivity=generation expoxy propane/(generation expoxy propane molal quantity+generation propane diols rubs That number+generation monomethyl ether molal quantity) × 100%.
Utility model beneficial effect
(1) paste state bed reactor is a kind of gas in bubbling form by being suspended with the liquid (slurries) of fine solid particle Layer, to realize the reactor of gas, liquid, solid phase reaction process.Compared to moving bed and fixed bed reactors, the biography of paste state bed reactor Heat is more effective than them, and temperature control is relatively easy.There is homogeneous temperature catalyst activity position in paste state bed reactor Degree, it is to avoid being emerged of focus.The utility model application bubble tower paste state bed reactor and the combination of tank diameter paste state bed reactor The technique of series connection carries out propylene ring oxidation reaction, and under this process conditions, epoxidation reaction is gentleer, and effectively overcoming should Strongly exothermic during epoxidation reaction and possible caused temperature runaway problem is carried out with moving bed or fixed bed reactors;
(2) it is that the method stirred using gas sparging makes catalyst particle keep outstanding in bubble tower paste state bed reactor It is floating;In tank diameter paste state bed reactor, catalyst particle is it is kept suspended state using churned mechanically method.Bubbling Tower paste state bed reactor does not have moving component, it is not necessary to which big power is used to stir, therefore bubble tower paste state bed reactor machinery Design is relatively easy, and liquid holdup is big, and running cost is relatively low;And although tank diameter paste state bed reactor needs to consider agitator Sealing problem, but it generally has higher heat transfer and mass-transfer efficiency.
The technique of the utility model application bubble tower paste state bed reactor and tank diameter paste state bed reactor combined serial is entered Row propylene ring oxidation reaction, under this process conditions, propylene ring oxidation reaction is mainly carried out in bubble tower paste state bed reactor, The conversion ratio of hydrogen peroxide reaches more than 80% in raw material.The hydrogen peroxide of residue about 20% enters tank diameter slurry bed system in raw material Reactor continues to participate in epoxidation reaction, high heat transfer, mass transfer characteristic based on tank diameter paste state bed reactor, residue about 20% Hydrogen peroxide almost all in tank diameter paste state bed reactor is converted, and the total conversion of hydrogen peroxide reaches more than 99%.
(3) major defect of paste state bed reactor has sizable back mixing for liquid phase, and liquid phase back mixing can cause catalytic reaction During side reaction generation.The utility model application bubble tower paste state bed reactor and tank diameter paste state bed reactor combination string The technique of connection carries out propylene ring oxidation reaction, and under this process conditions, liquid phase back mixing is inevitable.To avoid liquid phase back mixing from causing The generation of accessory substance, the utility model controls reaction pressure in 0.1~0.6MPa, preferably 0.3~0.6MPa.Relatively low operation pressure Air-liquid and solid phase propylene ring oxidation reaction are carried out under power, the generation of side reaction is effectively inhibited.Under this process conditions, raw material Effective rate of utilization >=95% of hydrogen peroxide, selectivity >=98% of product propene oxide, the total conversion of hydrogen peroxide is reachable To more than 99%.
Brief description of the drawings
Fig. 1 is process unit schematic diagram of the present utility model;
In figure, 1, bubble tower paste state bed reactor;2nd, sedimentation separation unit;3rd, tank diameter paste state bed reactor;4th, stir Groove paste state bed reactor II;
11st, methanol/hydrogen peroxide adds mouth;12nd, propylene adds mouth B;13rd, catalyst adds mouth C;14th, propylene outlet E; 15th, suspension slurry is exported;
21st, concentrated slurry is exported;22nd, purified liquor outlet;
31st, clear liquid adds mouth H;32nd, propylene adds mouth K;33rd, catalyst adds mouth I;34th, propylene outlet L;35th, metal film Separator-filter J.
41st, clear liquid adds mouth;42nd, propylene adds mouth;43rd, catalyst adds mouth;44th, propylene is exported;45th, metal UF membrane Filter.
Embodiment
The embodiments of technical solutions of the utility model is described in detail below, but the utility model be not limited to Lower description content:
Embodiment 1
As shown in figure 1, a kind of device for preparing expoxy propane, successively including bubble tower paste state bed reactor 1, sedimentation separation Unit 2, tank diameter paste state bed reactor 3, the bottom of bubble tower paste state bed reactor 1 add the He of mouth 11 provided with methanol/hydrogen peroxide Propylene adds mouth B12, and top adds mouth C13 and propylene outlet E14, the propylene outlet E14 connection tank diameters provided with catalyst The bottom propylene of paste state bed reactor 3 adds mouth K;The connection of suspension slurry outlet 15 of the middle and upper part of bubble tower paste state bed reactor 1 is heavy Separative element 2 drops;The bottom concentrated slurry outlet 21 of sedimentation separation unit 2 connects the bottom of bubble tower paste state bed reactor 1;Sedimentation point The bottom clear liquid of the connection tank diameter of purified liquor outlet 22 paste state bed reactor 3 from the middle and upper part of unit 2 adds mouth H31;Tank diameter slurry The top of bed reactor 3 exports L34 provided with propylene and catalyst adds mouth I33.The inside of tank diameter paste state bed reactor 3 is provided with metal UF membrane filter J35.
Also include tank diameter paste state bed reactor II 4, the propylene outlet E14, propylene add mouth K32, tank diameter slurry The bottom propylene of bed reactor II 4 adds mouth 42 and is interconnected;Purified liquor outlet 22, clear liquid add mouth H31, tank diameter slurry reactor The bottom clear liquid of device II 4 adds mouth 41 and is interconnected;The top of tank diameter paste state bed reactor II 4 is provided with propylene outlet 44 and catalyst Add mouth 43.The inside of tank diameter paste state bed reactor II 4 is provided with metal film separator-filter 45.
The method that expoxy propane is prepared using said apparatus:
(1) high strength titanium silicone zeolite molecular sieve microsphere is prepared
TS-1 zeolites are prepared using traditional hydrothermal synthesis method:By tetraethyl orthosilicate, butyl titanate, isopropanol, four SiO in gel, gel is obtained after propyl group ammonium hydroxide and deionized water solution mixing and stirring2:TiO2:TPAOH:H2O's rubs You are than being 1:0.025:0.3:25;The ethanol of isopropanol and hydrolysis generation is distilled off;Then gel is moved to polytetrafluoro In the Hydrothermal Synthesiss kettle of ethene, crystallization 48h at a temperature of 170 DEG C.By the product filtering after crystallization, fully washing, 110 DEG C of temperature Dried in the lower air atmosphere of degree and be calcined 3h in air atmosphere at a temperature of 12h, 550 DEG C, obtain nano-scale TS-1 zeolite.
Nano-scale TS-1 zeolite is dispersed in Ludox, then spray-dried that particle diameter is made is high-strength for 20~80 μm Spend microballoon.
(2) in bubble tower paste state bed reactor epoxidation reaction occurs for propylene and hydrogen peroxide
Mouth 11 is added from methanol/hydrogen peroxide appropriate solvent methanol is pumped into bubble tower paste state bed reactor 1;By being catalyzed Agent adds the high strength titanium silicon microspherical catalyst that mouth C adds 20~80 μm of the particle diameter prepared in (1).Adjust reactor temperature 40 ~50 DEG C, reaction pressure 0.45MPa.Mouth 11 is added from methanol/hydrogen peroxide mixing is pumped into bubble tower paste state bed reactor 1 Uniform methanol and hydrogen peroxide;Mouth B is added from propylene and is pumped into propylene into bubble tower paste state bed reactor 1.Raw material propylene, mistake Hydrogen oxide and solvent methanol are according to mol ratio 3:1:4.5 ratio is pumped into, and is started propylene ring oxidation reaction, is set up reaction cycle.
Reacted suspension slurry enters sedimentation separation unit 2 by outlet 15 in bubble tower paste state bed reactor 1, through heavy Isolated supernatant liquor (mainly comprising expoxy propane, methanol and hydrogen peroxide) and the concentrated slurry containing catalyst drop.In drum Steep unreacted gas-phase propene in tower paste state bed reactor 1 and export the tank diameter slurry reactor that E enters later procedure through propylene Epoxidation reaction is continued to participate in device 3 or tank diameter paste state bed reactor II 4.Supernatant liquor in sedimentation separation unit is through clear liquid Outlet 22, which is pumped into the tank diameter paste state bed reactor 3 or tank diameter paste state bed reactor II 4 of later procedure, to be continued to react, and is contained The concentrated slurry of catalyst then participates in reaction in the concentrated blowback bubble tower paste state bed reactor 1 of serum outlet 21 again.
After being reacted through bubble tower paste state bed reactor 1, conversion ratio >=80% of hydrogen peroxide in raw material.
(3) in tank diameter paste state bed reactor epoxidation reaction occurs for propylene and hydrogen peroxide
Mouth H31 is added from clear liquid or clear liquid adds mouth 41 to tank diameter paste state bed reactor 3 or tank diameter slurry reactor Appropriate methanol is pumped into device II 4, mouth I33 is added by catalyst or catalyst adds mouth 43 and adds the particle diameter 20 prepared in (1) ~80 μm of high strength titanium silicon microspherical catalyst.Adjust 40~50 DEG C of reactor temperature, reaction pressure 0.45MPa.Start anti- It should stir, into reactiveness.
Mouth H31 is added from clear liquid or clear liquid adds mouth 41 to tank diameter paste state bed reactor 3 or tank diameter slurry reactor Device II 4 is pumped into the clear liquid of the separation of sedimentation separation unit 2, adds mouth K32 from propylene or propylene adds mouth 42 to tank diameter slurry bed system Propylene is passed through in reactor 3 or tank diameter paste state bed reactor II 4, starts propylene ring oxidation reaction.React after 40min, stop The clear liquid of the separation of sedimentation separation unit 2 is pumped into, but still is passed through propylene and continues to react 20min.Altogether after reaction 60min, stop logical Enter propylene, stop stirring, epoxidation reaction is finished.Now, obtain containing epoxidation product (predominantly expoxy propane), solvent methanol With the mixed serum of catalyst.
Mixed serum is separated by filtration by metal film separator-filter J35 or metal film separator-filter 45 (mainly to include Expoxy propane, methanol and catalyst), the clear liquid (mainly comprising expoxy propane and methanol) filtered out is pumped into later separation process; And stayed in by the catalyst that metal film is retained in reactor and continue to participate in reaction.Unreacted propylene is by exporting L34 or propylene Later separation process is also entered by outlet 44.Propylene and methanol loop after being separated through separation circuit are utilized.
Tank diameter paste state bed reactor 3 and the alternately above-mentioned epoxidation reaction of tank diameter paste state bed reactor II 4 and mixed Close slurries lock out operation.When tank diameter paste state bed reactor 3 is carrying out propylene ring oxidation reaction, tank diameter paste state bed reactor 4 are carrying out the separation of mixed serum, and the interval time of two reactor blocked operations is 60min.
After agitated groove paste state bed reactor 3 or tank diameter paste state bed reactor II 4 reaction, hydrogen peroxide in reaction product Effective rate of utilization >=95%, selectivity >=98% of product propene oxide, total conversion >=99% of hydrogen peroxide.
Examples detailed above simply to illustrate technical concept of the present utility model and technical characterstic, can not limit this reality with this With new protection domain.All equivalent transformations done according to essence of the present utility model or modification, should all cover in this reality Within new protection domain.

Claims (4)

1. a kind of device for preparing expoxy propane, it is characterised in that successively including bubble tower paste state bed reactor, sedimentation separation list Member, tank diameter paste state bed reactor, bubble tower paste state bed reactor bottom adds mouth provided with methanol/hydrogen peroxide and propylene is added Mouth B, top adds mouth C and propylene outlet E provided with catalyst, and the propylene outlet E connects tank diameter paste state bed reactor bottom Propylene adds mouth K;The suspension slurry outlet connection sedimentation separation unit of bubble tower paste state bed reactor middle and upper part;Sedimentation separation list First bottom concentrated slurry outlet bubble tower paste state bed reactor bottom;Purified liquor outlet connection in the middle part of sedimentation separation unit is stirred Mix groove paste state bed reactor bottom clear liquid and add mouth H;L is exported provided with propylene and catalyst adds at the top of tank diameter paste state bed reactor Entrance I.
2. the device of expoxy propane is prepared according to claim 1, it is characterised in that also including tank diameter paste state bed reactor II, the propylene outlet E, propylene add mouth K, the bottom propylene of tank diameter paste state bed reactor II and add mouth and be interconnected;Clear liquid Outlet, clear liquid add mouth H, the bottom clear liquid of tank diameter paste state bed reactor II and add mouth and be interconnected;Tank diameter slurry reactor The top of device II adds mouth provided with propylene outlet and catalyst.
3. the device according to claim 1 or claim 2 for preparing expoxy propane, it is characterised in that in tank diameter paste state bed reactor Portion is provided with metal film separator-filter J.
4. the device of expoxy propane is prepared according to claim 2, it is characterised in that inside tank diameter paste state bed reactor II Provided with metal film separator-filter.
CN201621445741.1U 2016-12-27 2016-12-27 A kind of device for preparing expoxy propane Active CN206318907U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111724863A (en) * 2019-03-22 2020-09-29 中国石油化工股份有限公司 Method for predicting and controlling hydrogen peroxide conversion rate in preparation of propylene oxide by TS-1 method
CN115197171A (en) * 2021-04-13 2022-10-18 中国石油化工股份有限公司 Method and system for producing propylene oxide

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111724863A (en) * 2019-03-22 2020-09-29 中国石油化工股份有限公司 Method for predicting and controlling hydrogen peroxide conversion rate in preparation of propylene oxide by TS-1 method
CN111724863B (en) * 2019-03-22 2023-01-31 中国石油化工股份有限公司 Method for predicting and controlling hydrogen peroxide conversion rate in preparation of epoxypropane by TS-1 method
CN115197171A (en) * 2021-04-13 2022-10-18 中国石油化工股份有限公司 Method and system for producing propylene oxide

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