CN114425292A - Cumene hydroperoxide normal pressure tubular reactor and production process - Google Patents

Cumene hydroperoxide normal pressure tubular reactor and production process Download PDF

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Publication number
CN114425292A
CN114425292A CN202210117371.2A CN202210117371A CN114425292A CN 114425292 A CN114425292 A CN 114425292A CN 202210117371 A CN202210117371 A CN 202210117371A CN 114425292 A CN114425292 A CN 114425292A
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reactor
cumene hydroperoxide
air
air inlet
group
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陈春
陈曦
于淼
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Liaoning Fuqing Auxiliary Co ltd
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Liaoning Fuqing Auxiliary Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • B01J4/005Feed or outlet devices as such, e.g. feeding tubes provided with baffles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C407/00Preparation of peroxy compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/007Aspects relating to the heat-exchange of the feed or outlet devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00083Coils
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A cumene hydroperoxide normal pressure tubular reactor and a production process belong to the technical field of organic peroxide oxidation devices and production processes, the reactor comprises a reactor, a spiral tube heat exchanger, a condenser and a connecting pipeline, wherein the number of the reactor (11) is more than or equal to 2, the reactor groups are formed by flange interconnection, the number of the reactor groups is more than or equal to 4, a feed inlet is formed on the tube wall of the first reactor group on the left, a discharge outlet is formed on the tube wall of the first reactor group on the right, one end of the connected reactor group is connected with the condenser through a reactor connecting tube and a condenser connecting tube, an air distributor is arranged in the tube wall of the other end and is connected with an air inlet tube connecting tube through an air inlet tube connecting tube flange, the air inlet tube connecting tube is connected with an air inlet tube, the air inlet tube is connected with an air compressor, and the spiral tube heat exchanger is arranged in the reactor. The reactor of the invention has simple structure, low cost, convenient use and high production efficiency, the product purity can reach about 95 percent, and the safety of the equipment is obviously improved.

Description

Cumene hydroperoxide normal pressure tubular reactor and production process
The application is a divisional application of an invention patent with a parent case name of 'cumene hydroperoxide normal pressure tubular reactor and production process'; the parent application has the application number: CN 201710260741.7; the application date of the parent application is as follows: 2017.04.20.
Technical Field
The invention belongs to the technical field of organic peroxide oxidation devices and production processes, and particularly relates to a normal-pressure tubular reactor for generating cumene hydroperoxide by oxidation reaction of cumene and air and a production process.
Background
Cumene Hydroperoxide (CHP) is generated by air oxidation of cumene, which is the first step reaction of cumene hydroperoxide (DCP) by the cumene method and is also the most important reaction. The existing cumene oxidation reaction is greatly influenced by pH value. If the acidity in the reaction system is large, that is, the pH value is low, the oxidation reaction is unfavorable. Since the acidic material promotes the decomposition of CHP and the phenol product of the acid decomposition further inhibits the reaction. Therefore, the pH value needs to be controlled within a certain range, and the pH value is generally controlled to be 3-7 industrially. The acidic substances in the reaction system are mainly formic acid and benzoic acid generated by oxidation side reaction. Sometimes the carbon dioxide content in the air is increased, the atmosphere is polluted, or the fed cumene carries some acidic substances. In the oxidation production of cumene, in order to neutralize acidic substances, a gap or a continuous process is solved by intermittently and manually adding a certain amount of a low-concentration aqueous solution of alkali or an aqueous solution of basic salt (such as sodium carbonate) into an oxidation tower. The manual intermittent addition of alkali liquor has the problems of control lag, large alkali concentration fluctuation in an oxidation system, poor alkali addition regularity, incapability of accurately controlling the pH value of oxidation reaction oxidation liquid and the like, and meanwhile, the DCP condensation production process uses an acid catalyst, so that when the oxidation liquid is neutral or slightly alkaline, the condensation reaction speed is slowed, or even no reaction is caused.
At present, two main types of equipment are adopted for generating cumene hydroperoxide by an air oxidation reaction of cumene, and one type of equipment is a multi-tower type oxidation reactor adopted by U.S. Helcles company. The other is a large-volume tank type oxidation reactor adopted by American Global oil products company. Neither reactor is capable of removing acidic species generated during the oxidation reaction in time. The accumulation of acidic substances lowers the pH, and the oxidation reaction of cumene with air is inhibited, so that the concentration of the generated reactant can only reach about 20% at most. Secondly, because CHP is unstable and is decomposed by heat, the thermal decomposition is serious at 80 ℃, the thermal decomposition is more severe when the temperature is increased, and the oxidation liquid can not be concentrated by atmospheric distillation under the condition that an acid substance exists in a concentration system, so that explosion often occurs, and the safety of the two devices is required to be further improved. Thirdly, the two reactors have serious back mixing, high yield of byproducts which accounts for about 10 percent of the target product and poor selectivity. Fourthly, the air residence time is short and the oxygen utilization rate is low.
Disclosure of Invention
The invention aims to provide the cumene hydroperoxide oxidation reactor which has simple structure, low manufacturing cost, high production efficiency, good safety and normal pressure.
The purpose of the invention is realized by the following technical scheme:
the invention provides a cumene hydroperoxide normal pressure tubular reactor which comprises a plurality of reactor groups, wherein the plurality of reactor groups are connected with each other, and each reactor group comprises a plurality of connected reactors; a feed inlet is formed in the reactor group on the foremost side, a discharge outlet is formed in the reactor group on the rearmost side, and the reactor group is further connected with an air inlet pipe; the reactor is internally provided with a spiral tube heat exchanger, the reactor group is also connected with a condenser through a connecting pipeline, and the top end of the condenser is provided with a reaction gas outlet.
Preferably, the number of the reactor groups is at least four, and each reactor group comprises at least two reactors which are connected with each other through flanges.
Preferably, the reactor group is provided with four, and the front side is two between the reactor group and the rear side is two the reactor group all connects through a reactor connecting pipe, two the reactor connecting pipe pass through the condenser connecting pipe with the condenser is connected.
Preferably, a reaction material conveying pipe is connected between the pipe wall of the second reactor group from the left and the pipe wall of the second reactor group from the right.
Preferably, the bottom of the reactor group is connected with an air inlet pipe connecting pipe through an air inlet pipe connecting pipe flange, the air inlet pipe connecting pipe is connected with an air inlet pipe, and the air inlet pipe is connected with an air compressor; and the air inlet pipe connecting pipe is provided with a flowmeter.
Preferably, the spiral tube heat exchanger is connected with a heat source.
Preferably, an air distributor is arranged in the pipe wall of the reactor.
Preferably, the air distributor is uniformly perforated.
Preferably, a plurality of the air distributors and the spiral tube heat exchangers are arranged in the tube wall of the reactor, and the plurality of the air distributors and the plurality of the spiral tube heat exchangers are alternately arranged.
The invention also discloses a production process based on the cumene hydroperoxide normal pressure tubular reactor, which comprises the following steps:
pumping reaction materials into a reactor through a feed port by using a feed pump;
the air compressor presses air into the air inlet pipe and the air inlet pipe connecting pipe, and the air is uniformly distributed by the air distributor and then enters the reactor;
heating a heat exchange medium in the reactor through a spiral tube type heat exchanger, controlling the temperature to be 70-90 ℃, fully mixing reaction materials with air, and carrying out an oxidation reaction at normal pressure;
step four, cooling the acid gas generated by the oxidation reaction by a cooler and then discharging the cooled acid gas through a reaction gas discharge port;
step fifthly, discharging the generated reactant from a discharge hole after the multistage reaction.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the cumene hydroperoxide normal pressure tubular reactor has simple structure, low manufacturing cost and convenient use;
2. because the equipment can remove the acid gas generated in the oxidation reaction process in real time, and the reaction process is not inhibited, the production efficiency of the equipment is high, and the concentration of the oxidation reaction product can reach more than 40 percent and is improved by 100 percent compared with the original equipment;
3. the purity of alkaline cumene hydroperoxide obtained by concentrating and alkaline washing a crude product sent out by continuous reaction can reach about 95 percent and is improved by about 20 percent compared with the original equipment;
4. the reaction temperature of the oxidation reactor can be accurately controlled through the heat exchanger and the cooler of the reactor, so that the safety of the equipment is obviously improved;
5. almost no back-mixing occurs in the reactor, so the CHP has high purity and few impurities.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic representation of an atmospheric tubular reactor for cumene hydroperoxide of the present invention.
Figure 2 is a top plan view of an air distributor for an atmospheric tubular reactor for cumene hydroperoxide of the present invention.
In the figure: 1-air compressor, 2-flowmeter, 3-air distributor, 4-spiral tube heat exchanger, 5-condenser, 6-reactor connecting pipe, 7-air inlet pipe, 8-feed inlet, 9-discharge outlet, 10-reaction material conveying pipe, 11-reactor, 12-reaction gas discharge outlet, 13-condenser connecting pipe, 14-air inlet pipe connecting pipe, 15-air inlet pipe connecting pipe flange and 16-air distribution hole.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
As shown in figures 1-2, the invention provides a cumene hydroperoxide normal pressure tubular reactor which comprises a reactor 11, a spiral tube heat exchanger 4, a condenser 5 and a connecting pipeline. The reactor 11, the spiral tube heat exchanger 4 and the condenser 5 are connected through connecting pipelines. The number of the reactors 11 is 5, the reactors are connected with each other through flanges to form a reactor group, and one end of the reactor group formed after the connection is connected with the reactor connecting pipe 6 through the flanges. The other end of the reactor connection pipe 6 is connected to a condenser connection pipe 13 through a flange. The condenser connecting pipe 13 is connected with the condenser 5, and the top end of the condenser 5 is provided with a reaction gas exhaust port 12 for exhausting acid gas generated by oxidation reaction. The other end of the reactor group is provided with an air distributor 3 in the pipeline, and the air distributor 3 is uniformly provided with air distribution holes 16. The pipeline at the other end of the reactor group is connected with an air inlet pipe connecting pipe 14 through an air inlet pipe connecting pipe flange 15. The air inlet pipe connecting pipe 14 is connected with the air inlet pipe 7, and the air inlet pipe 7 is connected with the air compressor 1. The air distributor 3 is a metal plate made of a steel material. Holes for allowing air to pass through are uniformly formed in the metal plate, and the holes can uniformly distribute air input by the air compressor 1 in the tubular reactor group. The reactor 11 is internally provided with a spiral tube heat exchanger 4, and the spiral tube heat exchanger 4 is connected with a heat source. The pipe wall of the first reactor group on the left is provided with a feed inlet 8, and the number of the reactor groups is 4. The pipe wall of the first reactor group on the right is provided with a discharge port 9, and a reaction material conveying pipe 10 is connected between the pipe wall of the second reactor group on the left and the pipe wall of the second reactor group on the right. The intake pipe connection pipe 14 is provided with a flow meter 2 for measuring the flow rate of air in the intake pipe connection pipe 14.
The process steps of the invention when the cumene hydroperoxide normal pressure tubular reactor is produced are as follows:
pumping the reaction mass into a reactor 11 through a feed inlet 8 by a feed pump; the air compressor 1 presses air into the air inlet pipe 7 and the air inlet pipe connecting pipe 14, and the air is uniformly distributed by the air distributor 3 and then enters the reactor 11; in the reactor 11, a heat exchange medium is heated by a spiral tube heat exchanger 4, the temperature is controlled at 80 ℃, reaction materials are fully mixed with air, and oxidation reaction is carried out under normal pressure; acid gas generated by the oxidation reaction is cooled by a cooler 5 and then discharged through a reaction gas outlet; after passing through the multistage reaction, the resultant reactant is discharged from the discharge port 9.
Example 2
The number of the reactors 11 of the atmospheric pressure tubular cumene hydroperoxide reactor of the present invention was 6, the number of the reactor groups was 8, and the remaining parts and connection of the atmospheric pressure tubular cumene hydroperoxide reactor were the same as those of example 1.
The process of the invention for producing the cumene hydroperoxide normal pressure tubular reactor is that in the reactor 11, a heat exchange medium is heated by a spiral tube heat exchanger 4, the temperature is controlled at 70 ℃, reaction materials are fully mixed with air, and oxidation reaction is carried out under normal pressure, and the rest processes are the same as the process of the embodiment 1.
Example 3
The number of the reactors 11 of the atmospheric pressure tubular cumene hydroperoxide reactor of the present invention was 7, the number of the reactors was 12, and the remaining parts and connection of the atmospheric pressure tubular cumene hydroperoxide reactor were the same as those of example 1.
The process of the invention for producing the cumene hydroperoxide normal pressure tubular reactor is that in the reactor 11, a heat exchange medium is heated by a spiral tube heat exchanger 4, the temperature is controlled at 90 ℃, reaction materials are fully mixed with air, and oxidation reaction is carried out under normal pressure, and the rest processes are the same as the process of the embodiment 1.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (10)

1. Cumene hydroperoxide normal pressure tubular reactor, its characterized in that: the device comprises a plurality of reactor groups, wherein the reactor groups are connected with one another, and each reactor group comprises a plurality of connected reactors (11); a feed inlet (8) is formed in the foremost reactor group, a discharge outlet (9) is formed in the rearmost reactor group, and the reactor group is also connected with an air inlet pipe (7); the reactor (11) is internally provided with a spiral tube heat exchanger (4), the reactor group is also connected with a condenser (5) through a connecting pipeline, and the top end of the condenser (5) is provided with a reaction gas exhaust port (12).
2. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 1, wherein: the reactor group is provided with four at least, and each reactor group comprises at least two reactors (11) which are connected with each other through flanges.
3. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 2, wherein: the reactor group is provided with four, and the front side is two between the reactor group and the rear side is two the reactor group all connects through a reactor connecting pipe (6), two reactor connecting pipe (6) through condenser connecting pipe (13) with condenser (5) are connected.
4. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 3, wherein: a reaction material conveying pipe (10) is connected between the pipe wall of the second left reactor group and the pipe wall of the second right reactor group.
5. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 1, wherein: the bottom of the reactor group is connected with an air inlet pipe connecting pipe (14) through an air inlet pipe connecting pipe flange (15), the air inlet pipe connecting pipe (14) is connected with an air inlet pipe (7), and the air inlet pipe (7) is connected with an air compressor (1); and a flowmeter (2) is arranged on the air inlet pipe connecting pipe (14).
6. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 1, wherein: the spiral tube heat exchanger (4) is connected with a heat source.
7. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 1, wherein: an air distributor (3) is arranged in the pipe wall of the reactor (11).
8. The cumene hydroperoxide atmospheric pressure tubular reactor of claim 7, wherein: the air distributor (3) is uniformly provided with holes (16).
9. The cumene hydroperoxide atmospheric pressure tubular reactor according to claim 7 or 8, characterized in that: the reactor is characterized in that a plurality of air distributors (3) and the spiral tube heat exchangers (4) are arranged in the tube wall of the reactor (11), and the plurality of air distributors (3) and the plurality of spiral tube heat exchangers (4) are alternately arranged.
10. A process for the production of cumene hydroperoxide atmospheric pressure tubular reactor based on any one of claims 1 to 9 characterized in that: the method comprises the following steps:
pumping reaction materials into a reactor (11);
step II, inputting air into the reactor (11);
controlling the reaction temperature, fully mixing the reaction materials with air, and carrying out an oxidation reaction at normal pressure;
step four, discharging acid gas generated by oxidation reaction;
step fifthly, discharging the generated reactant from a discharge hole (9) after the multistage reaction.
CN202210117371.2A 2017-04-20 2017-04-20 Cumene hydroperoxide normal pressure tubular reactor and production process Pending CN114425292A (en)

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CN202210117371.2A CN114425292A (en) 2017-04-20 2017-04-20 Cumene hydroperoxide normal pressure tubular reactor and production process
CN201710260741.7A CN106905211A (en) 2017-04-20 2017-04-20 Isopropyl benzene hydroperoxide normal pressure tubular reactor and production technology

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CN201710260741.7A Division CN106905211A (en) 2017-04-20 2017-04-20 Isopropyl benzene hydroperoxide normal pressure tubular reactor and production technology

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CN114989777A (en) * 2022-06-22 2022-09-02 湖北绿新环保包装科技有限公司 Environment-friendly water-based transfer glue capable of improving firmness of paper

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