CN111072598B - Process for producing epichlorohydrin by direct oxidation of titanium-silicon molecular sieve catalyst - Google Patents
Process for producing epichlorohydrin by direct oxidation of titanium-silicon molecular sieve catalyst Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/08—Compounds containing oxirane rings with hydrocarbon radicals, substituted by halogen atoms, nitro radicals or nitroso radicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
- C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
Abstract
The invention provides a process for producing epoxy chloropropane by direct oxidation of a titanium silicon molecular sieve catalyst, which comprises the steps of pumping prepared methanol catalyst mixed solution and fresh chloropropene into a first mixer through a metering pump, mixing the mixed solution and hydrogen peroxide pumped into the first mixer, then feeding the mixed solution and the fresh chloropropene into a first tubular reactor for reaction, separating gas phase and liquid phase of a reaction product through a separator, mixing a separated liquid phase part with hydrogen peroxide fed into a second mixer, feeding the mixed solution into the second tubular reactor for reaction, feeding the reaction product into the second separator for gas-liquid separation, feeding the finally formed reaction product into a separating tank for separating a solid catalyst and a liquid phase product, pumping catalyst slurry into a batching tank for re-batching, and extracting the liquid product from a filter at the upper part of the separating tank.
Description
Technical Field
The invention belongs to the field of chemical product production technology, and relates to a process for producing epoxy chloropropane by direct oxidation of a titanium-silicon molecular sieve catalyst.
Background
The epichlorohydrin is an organic synthetic raw material and an intermediate with extremely strong functionality, and has very wide application. The method is used for preparing epoxy resin, glycerol, polyether polyol and the like, and is an important raw material for producing glycerol and glycidyl derivatives. Currently, the main processes for the preparation of epichlorohydrin include: propylene high temperature chlorination process, propylene acetate process, glycerin process, etc. Although these processes are technically mature, they all have unavoidable drawbacks such as: the method has the advantages of serious corrosion to equipment, high energy consumption, high requirement on raw material purity, more byproducts, large amount of generated wastewater, serious environmental damage and high investment cost of devices.
In order to overcome the above problems in the epichlorohydrin synthesis process, the scholars have studied a method for preparing epichlorohydrin by directly epoxidizing chloropropene.
US4833260 discloses a method for preparing epichlorohydrin by directly epoxidizing chloropropene with titanium-silicon molecular sieve as a catalyst and hydrogen peroxide as an oxidant. However, the epoxide formed will be partially subjected to ring-opening reaction due to the strong polar compounds present in the reaction system, which reduces the yield of the product. The epoxidation reaction of chloropropene is exothermic, if the released heat cannot be removed in time, the temperature of the system exceeds the control temperature, and the ineffective decomposition of hydrogen peroxide is increased, so that the effective utilization rate of the hydrogen peroxide is reduced. Based on this disadvantage, CN1219536a published 1999 adds a solid inert diluent to the catalyst to retard the reaction so that the reaction temperature is effectively controlled, but the effective volume of the reactor is significantly reduced.
CN201310211677.5 discloses a process for the oxidation of olefins by contacting an olefin and an oxidant with a catalyst on a fixed bed under olefin oxidation reaction conditions. The method can maintain the activity of the catalyst, the conversion rate of the oxidant and the selectivity of the target product at higher level in the reaction contact process, and prolong the one-way operation time of the catalyst, thereby delaying the deactivation of the catalyst and prolonging the service life of the catalyst. However, in the reaction process, the residence time of the reactant is insufficient, so that the effective contact area of the catalyst and the reactant is smaller, the reaction is not complete enough, and the yield per unit time is lower.
In order to improve the effective utilization rate of hydrogen peroxide, CN201110424544.7 discloses a method for continuously producing epichlorohydrin by direct epoxidation of chloropropene, wherein chloropropene, hydrogen peroxide, catalyst slurry and solvent are respectively conveyed into a reactor. A filter is arranged at the upper end of a discharge hole in the reactor to separate clear liquid containing products, the catalyst-containing unreacted complete material which is not filtered out at the lower end of the filter is returned to the reactor at the bottom end of the reactor. In the continuous production process, the catalyst is not required to be recovered, gas phase is condensed and reflowed through a condenser at the top of the reactor, and a jacket heat exchange layer is arranged outside the condenser and the reactor in the device, so that heat generated by the reaction can be exchanged and taken away, and the effective utilization rate of hydrogen peroxide is effectively improved. However, the hydrogen peroxide is fed once in the method, so that the conversion rate of chloropropene is not high, and the yield of epichlorohydrin is low.
CN200710046989.X discloses a method for producing epichlorohydrin by catalytic oxidation of chloropropene with hydrogen peroxide as oxidant and a fixed bed as reactor under the catalysis of titanium-silicon molecular sieve. The heat released in the reaction process is concentrated on the catalyst bed layer, so that the heat cannot be transferred or converted in time, the reaction temperature is unstable, and the selectivity of the epichlorohydrin is easily reduced.
Disclosure of Invention
In view of the defects in the prior art, the technical problems to be solved by the invention are as follows: the effective utilization rate of hydrogen peroxide is low, the catalyst is difficult to separate and recycle, the load of a process device is large, and the like. In order to achieve the aim, the invention provides a novel process method for producing epoxy chloropropane by directly oxidizing a titanium silicalite molecular sieve catalyst, which has the characteristics of stable reaction temperature, simple process flow, high yield of epoxy chloropropane, high effective utilization rate of hydrogen peroxide and the like.
In one aspect, the present invention provides an apparatus for producing epichlorohydrin, comprising a first mixer, a first tubular reactor, a first separator, a second mixer, a second tubular reactor, a second separator, a separator tank, and a filter;
the outlet of the first mixer is communicated with the feed inlet of the first tubular reactor through a pipeline;
the outlet of the first tubular reactor is communicated with the feed inlet of the first separator; the liquid phase outlet of the first separator is communicated with the feed inlet of the second mixer through a pipeline; the outlet of the second mixer is communicated with the feed inlet of the second tubular reactor through a pipeline; the outlet of the second tubular reactor is communicated with the feed inlet of the second separator; the liquid phase outlet of the second separator is communicated with the feed inlet of the separating tank;
the upper part of the separating tank is provided with a clear liquid discharging port; the filter is arranged at the discharge port of the clear liquid.
Based on the above technical solution, preferably, the apparatus further includes a first condenser and a second condenser; the first condenser is arranged at the top of the first separator; the second condenser is arranged at the top of the second separator.
The invention also provides a process for producing epoxy chloropropane by using the device and utilizing titanium-silicon molecular sieve catalyst to directly oxidize:
(1) Pumping fresh chloropropene and solvent methanol added with a catalyst into a first mixer through a metering pump, uniformly mixing the fresh chloropropene and the solvent methanol with the catalyst into the first mixer through the metering pump, and conveying the mixture to a first tubular reactor for reaction after mixing; the temperature of the first tubular reactor is 20-70 ℃ and the residence time is 1-7h;
(2) The materials after the reaction of the first tubular reactor enter a first separator through an outlet, and nitrogen is introduced into the first separator, so that the pressure of the first separator is kept at 0.1-0.8MPa; the gas phase part enters a first condenser to be condensed and refluxed, the liquid phase part is conveyed to a second mixer through an outlet by a pump, and hydrogen peroxide aqueous solution is added into the second mixer again; conveying the reaction materials in the second mixer to a second tubular reactor for reaction; setting the temperature of the second tubular reactor to be 20-70 ℃ and the residence time to be 1-7h;
(3) The materials after the reaction of the second tubular reactor enter a second separator, nitrogen is introduced into the second separator, the pressure of the second separator is kept at 0.1-0.8MPa, and the gas phase part in the second separator enters a condenser above the second separator for condensation reflux;
(4) The final reaction product is pumped into a separating tank through a metering pump, a built-in filter is arranged at the upper part of the separating tank, the solid catalyst and the liquid phase product can be separated, the catalyst slurry is pumped into a batching tank through a pump to be re-batched, and the liquid phase product is extracted from the filter at the upper part of a settling tank.
Based on the technical scheme, preferably, the tubular reactor is a metal hollow tube with a smooth inner wall, the inner diameter is 10-500mm, and the length is 1-100m.
Based on the technical scheme, the weight and solid content percentage of the catalyst of the reaction liquid in the tubular reactor is preferably 0.1-30%; the mole number of hydrogen peroxide of the hydrogen peroxide aqueous solution added into the first mixer and the second mixer is 1/8-1 of that of chloropropene, and the two addition amounts of the hydrogen peroxide aqueous solution can be the same or different; the mass concentration of the chloropropene is more than 98%, the mass concentration of the hydrogen peroxide aqueous solution is 27% -70%, and the mass dosage ratio of the solvent methanol to the chloropropene is 0.1-5:1.
Based on the technical scheme, preferably, the filter is a ceramic membrane filter or a polytetrafluoroethylene filter element, and the pore diameter of the filter is 2-10 mu m smaller than the particle diameter of the catalyst; the filter is connected with the clear liquid discharging port in a detachable pipeline.
Based on the technical scheme, preferably, the filter is a polytetrafluoroethylene filter element; the pores of the polytetrafluoroethylene filter element are 1-50 mu m, the filter is composed of 1-100 polytetrafluoroethylene filter elements, and the polytetrafluoroethylene filter element is in a solid cylinder shape.
Based on the above technical scheme, preferably, the first condenser, the second condenser, the first tubular reactor and the second tubular reactor are all provided with jacket heat exchange layers.
Based on the technical scheme, preferably, the raw materials of the method further comprise an additive M 2 CO 3 Or MHCO 3 The M is K + 、Na + 、NH 4 + 。
Advantageous effects
(1) The front part of each tubular reactor is connected with a mixer, and the reaction materials in the tubular reactors are fully and uniformly mixed by the mixer before entering, so that the catalyst and the reaction materials are fully contacted, and the catalytic reaction is facilitated. Compared with the stirred tank reaction, the method reduces the energy consumption of the mixed materials and ensures stable reaction.
(2) The hydrogen peroxide aqueous solution enters the reaction materials in two steps respectively, so that the free regulation and control of the mole ratio of chloropropene to hydrogen peroxide can be realized, the self-decomposition reaction of hydrogen peroxide when meeting a catalyst is reduced, the effective utilization rate of hydrogen peroxide is improved, the production cost is reduced, and the working efficiency is improved.
(3) The invention designs two tubular reactors, which can effectively control the reaction temperature and the chloropropene conversion rate and increase the reaction safety.
(4) The separation tank is favorable for separating the catalyst, so that liquid phase is conveniently extracted through the filter element, the sedimentation of the solid catalyst can effectively reduce the load of the filter element, and the separation of the catalyst is facilitated.
(5) The load of the whole process device can be adjusted by adding a fresh chloropropene feeding pipeline, and the influence on the reaction process is reduced by adjusting the reaction time. The invention has potential market value.
Drawings
FIG. 1 is a schematic diagram of the process flow for producing epichlorohydrin according to the invention,
FIG. 2 is a schematic illustration of a process flow for producing epichlorohydrin in contrast to the present invention; wherein: p-1, P-2, P-3, P-4 and P-5 are all metering pumps, M-1 is a first mixer, R-1 is a first tubular reactor, V-1 is a first separator, L-1 is a first condenser, V-2 is a second separator, L-2 is a second condenser, M-2 is a second mixer, R-2 is a second tubular reactor, C is a separation tank, and F is a filter.
The present invention will be further illustrated by the following specific examples, but the scope of the present invention is not limited to the examples.
Detailed Description
The catalyst used in the present invention was a titanium silicalite catalyst prepared using the method disclosed in 201711344584.4. The method adopts the solid meta-titanic acid and the solid orthotitanic acid as titanium sources to synthesize the TS-1, alcohol substances are not needed to be added in the process of introducing new titanium, a certain burden is reduced for the subsequent alcohol removal step, and the meta-titanic acid and the orthotitanic acid are low in price, so that the synthesis cost can be reduced, and the production cost of the method is further saved.
Comparative example 1
According to the process for producing epichlorohydrin shown in figure 1.
Two tubular reactors are arranged, and the two tubular reactors are provided with heat exchange jacket layers so as to exchange heat generated by the reaction and take away the heat; the front parts of the two tubular reactors are provided with mixers so that the raw materials are fully mixed; reflux condensers are arranged at the tops of the two separators.
Fresh chloropropene and methanol added with a catalyst are pumped into a first mixer M-1 through a metering pump P-1, mixed with hydrogen peroxide pumped into the first mixer M-1 through a metering pump P-2, and conveyed to a first tubular reactor R-1 for reaction after being uniformly mixed. The mass ratio of the methanol to the chloropropene is 1:1, the mole number of hydrogen peroxide in the hydrogen peroxide is 1/6 of that of the chloropropene, the mass concentration of the hydrogen peroxide is 50%, the weight and solid content of the catalyst is 10%, no additive is added into the catalyst, and the feeding flow is 5L/h.
The material after the reaction of the first tubular reactor R-1 enters a first separator V-1, nitrogen is introduced from the outside above the liquid phase of the first separator V-1 to enable the pressure of the first separator V-1 to be kept at 0.4MPa, a gas phase part enters a first condenser L-1 at the top of the first separator V-1 to be condensed and refluxed, the liquid phase part is conveyed to a second mixer M-2 through a metering pump P-3 and conveyed to the second mixer M-2 together with hydrogen peroxide which is conveyed to the second mixer M-2 through a metering pump P-4 to be mixed, and the mixed material is conveyed to the second tubular reactor R-2 to be reacted together after being uniformly mixed, wherein the mole number of hydrogen peroxide in the hydrogen peroxide is 1/6 of that of chloropropene.
The material after the reaction of the second tubular reactor R-2 enters a second separator V-2, nitrogen is introduced from the outside into the liquid phase upper part of the second separator V-2, so that the pressure inside the second separator V-2 is maintained at 0.4MPa, and the gas phase part in the second separator V-2 enters a second condenser L-2 above the second separator V-2 for condensation reflux.
The materials pumped by the second separator V-2 are pumped into a separating tank C through a metering pump P-5, a built-in filter F is arranged at the upper part of the separating tank C, the solid catalyst and the liquid phase products can be separated, the catalyst slurry is pumped into a batching tank through a pump to be re-batched, and the liquid phase products are extracted from the filter F at the upper part of the separating tank C.
The reaction was continuously carried out for 1000 hours, and the separated clear liquid was analyzed to obtain the selectivity of epichlorohydrin and the effective utilization rate of hydrogen peroxide, as shown in table 1.
TABLE 1 partial reaction conditions and reaction results for comparative example 1
Comparative example 2
According to the process for producing epichlorohydrin shown in figure 2.
Two tubular reactors are arranged, and the two tubular reactors are provided with heat exchange jacket layers so as to exchange heat generated by the reaction and take away the heat; the front parts of the two tubular reactors are provided with mixers so that the raw materials are fully mixed; reflux condensers are arranged at the tops of the two separators.
Fresh chloropropene and methanol added with a catalyst are pumped into a first mixer M-1 through a metering pump P-1, mixed with hydrogen peroxide pumped into the first mixer M-1 through a metering pump P-2, and conveyed to a first tubular reactor R-1 for reaction after being uniformly mixed. The mass ratio of the methanol to the chloropropene is 1:1, the mol ratio of the chloropropene to the hydrogen peroxide is 3:1, the mass concentration of the hydrogen peroxide is 50%, the weight and solid content of the catalyst is 10%, and the additive Na is 2 CO 3 The amount of the catalyst was 15ppm based on the amount of the mixed liquor, and the feed rate was 5L/h.
The material after the reaction of the first tubular reactor R-1 enters a first separator V-1, nitrogen is introduced from the outside into the upper part of the liquid phase of the first separator V-1 to keep the pressure of the first separator V-1 at 0.4MPa, the gas phase part enters a first condenser L-1 at the top of the first separator V-1 to be condensed and refluxed, and the liquid phase part is conveyed into a second tubular reactor R-2 through a metering pump P-3. .
The material of the second tubular reactor R-2 enters a second separator V-2, nitrogen is introduced from the outside into the liquid phase above the second separator V-2, so that the pressure inside the second separator V-2 is maintained at 0.4MPa, and the gas phase part in the second separator V-2 enters a second condenser L-2 above the second separator V-2 for condensation reflux.
The materials pumped by the second separator V-2 are pumped into a separating tank C through a metering pump P-5, a built-in filter F is arranged at the upper part of the separating tank C, the solid catalyst and the liquid phase products can be separated, the catalyst slurry is pumped into a batching tank through a pump to be re-batched, and the liquid phase products are extracted from the filter F at the upper part of the separating tank C.
The reaction was continuously carried out for 1000 hours, and the separated clear liquid was analyzed to obtain the selectivity of epichlorohydrin and the effective utilization rate of hydrogen peroxide, as shown in table 2.
TABLE 2 partial reaction conditions and reaction results of comparative example 2
Example 1
According to the process for producing epichlorohydrin shown in figure 1.
Two tubular reactors are arranged, and the two tubular reactors are provided with heat exchange jacket layers so as to exchange heat generated by the reaction and take away the heat; the front parts of the two tubular reactors are provided with mixers so that the raw materials are fully mixed; reflux condensers are arranged at the tops of the two separators.
Fresh chloropropene and methanol added with a catalyst are pumped into a first mixer M-1 through a metering pump P-1, mixed with hydrogen peroxide pumped into the first mixer M-1 through a metering pump P-2, and conveyed to a first tubular reactor R-1 for reaction after being uniformly mixed. The mass ratio of the methanol to the chloropropene is 1:1, and the hydrogen peroxide isThe mole number of the hydrogen peroxide is 1/6 of that of chloropropene, the mass concentration of the hydrogen peroxide is 50%, the weight and solid content of the catalyst is 10%, and the additive Na is 2 CO 3 The amount of the catalyst was 15ppm based on the amount of the mixed liquor, and the feed rate was 5L/h.
The material after the reaction of the first tubular reactor R-1 enters a first separator V-1, nitrogen is introduced from the outside above the liquid phase of the first separator V-1 to enable the pressure of the first separator V-1 to be kept at 0.4MPa, a gas phase part enters a first condenser L-1 at the top of the first separator V-1 to be condensed and refluxed, the liquid phase part is conveyed to a second mixer M-2 through a metering pump P-3 and conveyed to the second mixer M-2 together with hydrogen peroxide which is conveyed to the second mixer M-2 through a metering pump P-4 to be mixed, and the mixed material is conveyed to the second tubular reactor R-2 to be reacted together after being uniformly mixed, wherein the mole number of hydrogen peroxide in the hydrogen peroxide is 1/6 of that of chloropropene.
The material after the reaction of the second tubular reactor R-2 enters a second separator V-2, nitrogen is introduced from the outside into the liquid phase upper part of the second separator V-2, so that the pressure inside the second separator V-2 is maintained at 0.4MPa, and the gas phase part in the second separator V-2 enters a second condenser L-2 above the second separator V-2 for condensation reflux.
The materials pumped by the second separator V-2 are pumped into a separating tank C through a metering pump P-5, a built-in filter F is arranged at the upper part of the separating tank C, the solid catalyst and the liquid phase products can be separated, the catalyst slurry is pumped into a batching tank through a pump to be re-batched, and the liquid phase products are extracted from the filter F at the upper part of the separating tank C.
The reaction was continuously carried out for 1000 hours, and the separated clear liquid was analyzed to obtain the selectivity of epichlorohydrin and the effective utilization rate of hydrogen peroxide, as shown in table 3.
TABLE 3 partial reaction conditions and reaction results for example 1
As can be seen by comparing the results of tables 1 and 3, additive Na 2 CO 3 The addition of (3) can improve the activity of the catalyst. The selectivity of the epichlorohydrin is kept at about 99 percent and the highest value reaches 99.6 percent after the continuous reaction is carried out for 1000 hours, which is higher than the condition without additives; the effective utilization rate of hydrogen peroxide is maintained above 98%, and the highest value is 98.7%. The catalyst has high activity and stability under the condition of adding the additive.
As can be seen from comparing the results of table 2 and table 3, the hydrogen peroxide is added in two times, and the effective utilization rate of hydrogen peroxide can be significantly improved. The effective utilization rate of hydrogen peroxide is maintained above 98% and the highest value reaches 98.7% after continuous reaction for 1000 hours. Compared with the two-time addition of the hydrogen peroxide and the one-time addition of the hydrogen peroxide, the selectivity of the epichlorohydrin and the effective utilization rate of the hydrogen peroxide are both obviously improved.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention in any way.
Claims (5)
1. A method for producing epichlorohydrin, characterized by using an apparatus for producing epichlorohydrin;
the device comprises a first mixer, a first tubular reactor, a first separator, a second mixer, a second tubular reactor, a second separator, a separation tank and a filter;
the outlet of the first mixer is communicated with the feed inlet of the first tubular reactor through a pipeline;
the outlet of the first tubular reactor is communicated with the feed inlet of the first separator; the liquid phase outlet of the first separator is communicated with the feed inlet of the second mixer through a pipeline; the outlet of the second mixer is communicated with the feed inlet of the second tubular reactor through a pipeline; the outlet of the second tubular reactor is communicated with the feed inlet of the second separator; the liquid phase outlet of the second separator is communicated with the feed inlet of the separating tank;
the upper part of the separating tank is provided with a clear liquid discharging port; the filter is arranged at the clear liquid discharge port;
the apparatus further comprises a first condenser and a second condenser; the first condenser is arranged at the top of the first separator; the second condenser is arranged at the top of the second separator;
the method comprises the following steps:
(1) Pumping fresh chloropropene and solvent methanol added with a catalyst into a first mixer through a metering pump, uniformly mixing the fresh chloropropene and the solvent methanol with the catalyst into the first mixer through the metering pump, and conveying the mixture to a first tubular reactor for reaction after mixing; setting the reaction temperature of the first tubular reactor to be 20-70 ℃ and the residence time to be 1-7h;
(2) The reaction materials in the first tubular reactor enter a first separator through an outlet, nitrogen is introduced into the first separator, and the pressure of the first separator is kept between 0.1 and 0.8MPa; the gas phase part enters a first condenser to be condensed and refluxed, the liquid phase part is conveyed to a second mixer through an outlet by a pump, hydrogen peroxide water solution is added into the second mixer, the reaction materials in the second mixer are conveyed to a second tubular reactor to react, the reaction temperature of the second tubular reactor is set to be 20-70 ℃, and the residence time is set to be 1-7h; the reacted reaction material enters a second separator through an outlet, and nitrogen is introduced into the second separator, so that the pressure of the second separator is kept at 0.1-0.8MPa; the gas phase part enters a second condenser to be condensed and refluxed, the liquid phase part is conveyed to a separating tank through an outlet by a pump, and clear liquid containing the product is separated out by a filter of a clear liquid outlet;
the catalyst is a titanium silicalite molecular sieve catalyst, and the raw materials of the method comprise an additive M 2 CO 3 Or MHCO 3 The M is K + 、Na + 、NH 4+ ；
The weight and solid content percentage of the catalyst of the reaction liquid in the tubular reactor is 0.1-30 percent; the mole numbers of the hydrogen peroxide in the hydrogen peroxide aqueous solution added into the first mixer and the second mixer are 1/8-1 of the mole number of the chloropropene, and the two hydrogen peroxide aqueous solutions are added in the same or different amounts; the mass concentration of the chloropropene is more than 98%, the mass concentration of the hydrogen peroxide aqueous solution is 27% -70%, and the mass dosage ratio of the solvent methanol to the chloropropene is 0.1-5:1.
2. The method according to claim 1, wherein the tubular reactor is a metal hollow tube with a smooth inner wall, an inner diameter of 10-500mm and a length of 1-100m.
3. The method according to claim 1, wherein the filter is a ceramic membrane filter or a polytetrafluoroethylene filter element, and the pore size of the filter is 2-10 μm smaller than the particle size of the catalyst; the filter is connected with the clear liquid discharging port in a detachable pipeline.
4. The method of claim 1, wherein the filter is a polytetrafluoro-filter cartridge; the pores of the polytetrafluoroethylene filter element are 1-50 mu m, the filter is composed of 1-100 polytetrafluoroethylene filter elements, and the polytetrafluoroethylene filter element is in a solid cylinder shape.
5. The method according to claim 1, wherein the first condenser, the second condenser, the first tubular reactor and the second tubular reactor are each provided with a jacket heat exchange layer.
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| CN107879998A (en) * | 2017-10-26 | 2018-04-06 | 河北美邦工程科技股份有限公司 | A kind of segmented propylene oxide process |
| CN109912541A (en) * | 2019-02-26 | 2019-06-21 | 山东凯泰科技股份有限公司 | A kind of realized using phase transfer catalyst directly produces ECH continuous production commercial run |
| CN110078683A (en) * | 2019-05-20 | 2019-08-02 | 江苏扬农化工集团有限公司 | A kind of epoxychloropropane is continuously synthesizing to technique |
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| CN111072598A (en) | 2020-04-28 |
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