CN106905211A - Atmospheric pressure tubular reactor for cumene hydrogen peroxide and its production process - Google Patents

Abstract

A normal pressure tubular reactor for cumene hydroperoxide and its 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, and is characterized in that 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 from the left, a discharge outlet is formed on the tube wall of the first reactor group from 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, the connected reactor group 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. 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

Atmospheric pressure tubular reactor for cumene hydrogen peroxide and its production process

technical field

The invention belongs to the technical field of an organic peroxide oxidation device and a production process, and in particular relates to an atmospheric pressure tubular reactor and a production process for generating cumene hydrogen peroxide through the oxidation reaction of cumene and air.

Background technique

Cumene air oxidation reaction generates cumene hydroperoxide (CHP for short), is the first step reaction of cumene method to produce cumene peroxide (DCP), is also the most important reaction. The existing cumene oxidation reaction is greatly affected by the pH value. If the acidity in the reaction system is high, that is, the pH value is low, it is very unfavorable for the oxidation reaction. Because acidic substances will promote the decomposition of CHP, and the product of acid decomposition, phenol, further inhibits the reaction. Therefore, it is necessary to control the pH value within a certain range. Generally, the pH value is controlled in the industry to be 3-7. The acidic substances in the reaction system are mainly formic acid and benzoic acid generated by oxidation side reactions. Sometimes the carbon dioxide content in the air increases, air pollution, or some acidic substances in the feed cumene. In the oxidation production of cumene, in order to neutralize acidic substances, a certain amount of low-concentration alkaline aqueous solution or basic salt (such as sodium carbonate) aqueous solution is artificially added to the oxidation tower intermittently or intermittently during the oxidation process. to be resolved. Artificial intermittent addition of lye has problems such as control lag, large fluctuations in alkali concentration entering the oxidation system, poor alkali addition regularity, and inability to accurately control the pH value of the oxidizing solution in the oxidation reaction. At the same time, the DCP condensation production process uses an acidic catalyst. Alkalinity or alkalinity will also cause the condensation reaction to slow down, or even not react.

At present, there are mainly two types of equipment used in the air oxidation reaction of cumene to generate cumene hydroperoxide. One is the multi-tower oxidation reactor adopted by the U.S. Helcles company. The other is the large-volume tank-type oxidation reactor used by Universal Oil Company of the United States. Neither of the two reactors can remove the acidic substances generated during the oxidation reaction from the reactor in time. The accumulation of acidic substances reduces the pH value, which inhibits the oxidation reaction of cumene and air, so that the concentration of the generated reactants can only reach about 20% at most. Second, because CHP is unstable and thermally decomposes, the thermal decomposition is serious at 80°C, and when the temperature rises, the thermal decomposition is more severe. In the case of acidic substances in the enrichment system, explosions often occur because of this , Therefore, the oxidizing solution cannot be concentrated by atmospheric distillation, and the safety of the two devices needs to be further improved. Third, the above two reactors are seriously backmixed, and the yield of by-products is high, accounting for about 10% of the target product, and the selectivity is poor. Fourth, the air residence time is short and the oxygen utilization rate is low.

Contents of the invention

The purpose of this invention is to provide a kind of simple in structure, with low cost, high production efficiency, good safety, the cumene hydroperoxide oxidation reactor that uses under normal pressure.

The purpose of the present invention is achieved by the following technical solutions: cumene hydrogen peroxide atmospheric pressure tubular reactor, comprising reactor, spiral tube heat exchanger, condenser, connecting pipeline, said reactor, spiral tube The heat exchanger and the condenser are connected by connecting pipes, which are characterized in that the said reactors are ≥ 2, and are connected to each other by flanges to form a reactor group, and the reactor groups are ≥ 4, and the tube of the first reactor group from the left There is a feed inlet on the wall, and a discharge outlet on the tube wall of the first reactor group from the right. One end of the connected reactor group is connected to the condenser through the reactor connecting pipe and the condenser connecting pipe, and the other end An air distributor is installed in the wall of the pipe, which is connected to the inlet pipe connecting pipe through the inlet pipe connecting pipe flange, the inlet pipe connecting pipe is connected to the inlet pipe, the inlet pipe is connected to the air compressor, and the top of the said condenser is equipped with a reaction Gas outlet, the reactor is equipped with a spiral tube heat exchanger.

Further, it is characterized in that 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, and a flow meter is installed on the connecting pipe of the inlet pipe. .

Still further, it is characterized in that the air distributor is evenly formed with holes.

The production technique of cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention is characterized in that:

⑴. Use the feed pump to pump the reaction materials into the reactor through the feed port;

⑵. The air compressor presses the air into the inlet pipe and the inlet pipe connecting pipe, and the air is evenly distributed by the air distributor before entering the reactor;

⑶. In the reactor, the heat exchange medium is heated by a spiral tube heat exchanger, the temperature is controlled at 70-90°C, the reaction material is fully mixed with air, and the oxidation reaction is carried out under normal pressure;

(4) The acid gas generated by the oxidation reaction is cooled by the cooler and then discharged through the reaction gas outlet;

⑸. After passing through the multi-stage reaction, the generated reactants are discharged from the outlet.

The present invention has realized following beneficial effect:

1. The cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention is simple in structure, cheap in cost, easy to use;

2. Because the equipment can remove the acid gas generated during the oxidation reaction in real time, the reaction process will not be inhibited, so the production efficiency of the equipment is high, and the concentration of the oxidation reaction product can reach more than 40%, which is 100% higher than the original equipment;

3. The purity of alkaline cumene hydroperoxide can reach about 95%, which is about 20% higher than that of the original equipment;

4. Since the reaction temperature of the oxidation reactor can be precisely controlled through the heat exchanger and cooler of the reactor, the safety of the equipment is significantly improved;

5. There is almost no back-mixing phenomenon in the reactor, so CHP has high purity and less impurities.

Description of drawings

Fig. 1 is the schematic diagram of cumene hydroperoxide atmospheric pressure tubular reactor of the present invention.

Fig. 2 is the top view of the air distributor of the cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention.

In the picture: 1-air compressor, 2-flow meter, 3-air distributor, 4-coil heat exchanger, 5-condenser, 6-reactor connecting pipe, 7-intake pipe, 8-feed 9- outlet, 10- reaction material delivery pipe, 11- reactor, 12- reaction gas outlet, 13- condenser connecting pipe, 14- inlet pipe connecting pipe, 15- inlet pipe connecting pipe flange, 16- Air distribution holes.

Embodiments of the present invention will be described below in conjunction with the accompanying drawings.

detailed description

Example 1

The cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention comprises a reactor 11, a spiral tube heat exchanger 4, a condenser 5, and connecting pipelines. Said reactor 11, spiral tube heat exchanger 4, and condenser 5 are connected through connecting pipelines. There are five reactors 11, which are connected to each other through flanges to form a reactor group, and one end of the formed reactor group is connected to the reactor connecting pipe 6 through a flange. The other end of the reactor connecting pipe 6 is connected with the condenser connecting pipe 13 through a flange. The condenser connecting pipe 13 is connected with the condenser 5, and the top of the condenser 5 is equipped with a reaction gas outlet 12 for removing the acid gas generated by the oxidation reaction. The pipeline at the other end of the reactor group is equipped with an air distributor 3, and the air distributor 3 is evenly formed with air distribution holes 16. The pipeline at the other end of the reactor group is connected to the inlet pipe connecting pipe 14 through the inlet pipe connecting pipe flange 15 . The intake pipe connecting pipe 14 is connected with the intake pipe 7, and said intake pipe 7 is connected with the air compressor 1. The air distributor 3 is a metal plate made of steel material. The metal plate is evenly formed with holes that can pass through the gas, and the holes can evenly distribute the air input by the air compressor 1 in the tubular reactor group. The reactor 11 is equipped with a spiral tube heat exchanger 4, and the spiral tube heat exchanger 4 is connected with a heat source. The tube wall of the first reactor group on the left is shaped on feed inlet 8, and said reactor group is 4. The pipe wall of the first reactor group from the right is formed with a discharge port 9, and the pipe wall of the second reactor group from the left and the pipe wall of the second reactor group from the right are connected with a reaction material conveying pipe 10. Said inlet pipe connecting pipe 14 is equipped with a flow meter 2 for measuring the air flow in the inlet pipe connecting pipe 14 .

The process steps during the production of the cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention are: the reaction material is pumped into the reactor 11 by the feed port 8 with the feed pump; the air compressor 1 presses air into the intake pipe 7 and the inlet pipe connecting pipe 14, the air is uniformly distributed by the air distributor 3 and then enters the reactor 11; in the reactor 11, the heat exchange medium is heated by the spiral tube heat exchanger 4, and the temperature is controlled at 80°C. The air is fully mixed, and the oxidation reaction is carried out under normal pressure; the acid gas generated by the oxidation reaction is cooled by the cooler 5 and discharged through the reaction gas discharge port; after the multi-stage reaction, the generated reactants are discharged from the discharge port 9.

Example 2

The reactor 11 of the cumene hydrogen peroxide atmospheric tubular reactor of the present invention is 6, and the reactor group is 8, and the remaining parts and the connection mode of the cumene hydrogen peroxide atmospheric tubular reactor and implementation Example 1 is the same.

The production process of the cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention is in the reactor 11, the heat exchange medium is heated by the spiral tube heat exchanger 4, the temperature is controlled at 70°C, and the reaction materials are fully mixed with the air , Carry out oxidation reaction under normal pressure, all the other processes are identical with embodiment 1.

Example 3

The reactor 11 of the cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention is 7, and the reactor group is 12, and the remaining parts of the cumene hydrogen peroxide atmospheric pressure tubular reactor and the connection method and implementation Example 1 is the same.

The production process of the cumene hydrogen peroxide atmospheric pressure tubular reactor of the present invention is in the reactor 11, the heat exchange medium is heated by the spiral tube heat exchanger 4, the temperature is controlled at 90 ° C, and the reaction materials are fully mixed with the air , Carry out oxidation reaction under normal pressure, all the other processes are identical with embodiment 1.

Claims (4)

1. isopropyl benzene hydroperoxide normal pressure tubular reactor, including reactor (11), spiral tube exchanger（4）, condenser（5）, Connecting line, described reactor (11), spiral tube exchanger（4）, condenser（5）Connected by connecting line, its feature exists In described reactor（11）>=2, reactor group is interconnected to form with flange, reactor group >=4, left number first is anti- Charging aperture is formed with the tube wall for answering device group（8）, discharging opening is formed with first tube wall of reactor group of right number（9）, after connection Reactor group one end passes through reactor connecting tube（6）With condenser connecting tube（13）With condenser（5）Connection, the tube wall of the other end Built with air distributor（3）, by air inlet pipe connected pipe flange（15）With air inlet pipe connected pipe（14）Connection, air inlet pipe connection Pipe（14）With air inlet pipe（7）Connection, air inlet pipe（7）With air compressor machine（1）Connection, described condenser（5）Top equipped with reaction Gas outlet（12）, reactor（11）Built with spiral tube exchanger（4）.

2. such as described isopropyl benzene hydroperoxide normal pressure tubular reactor in claim 1, it is characterised in that described left number the Reaction mass delivery pipe is connected between two second reactor group tube walls of tube wall and right number of reactor group（10）, it is described Air inlet pipe connected pipe（14）It is upper that flowmeter is housed（2）.

3. such as isopropyl benzene hydroperoxide normal pressure tubular reactor described in claim 1 or 2, it is characterised in that described air Distributor（3）On be equably formed with hole（16）.

4. the production technology of isopropyl benzene hydroperoxide normal pressure tubular reactor of the present invention, it is characterised in that：

(1) passes through charging aperture with feed pump（8）Reaction mass is pumped into reactor（11）；

(2) air compressor machines（1）Air is pressed into air inlet pipe（7）With air inlet pipe connected pipe（14）, through air distributor（3）Air is equal Enter reactor after even distribution（11）；

(3) is in reactor（11）Interior, heat transferring medium passes through spiral tube heat exchanger（4）Heating, temperature control at 70-90 DEG C, instead Answer material to be sufficiently mixed with air, oxidation reaction is carried out at ambient pressure；

(4) the sour gas of oxidation reactions generation is through cooler（5）Pass through reaction gas outlet after cooling（12）Discharge；

(5) is by after reaction of high order, and the reactant of generation is from discharging opening（9）Discharge.