Preparation device and technological process of diisopropylbenzene hydroperoxide

Abstract

The invention discloses a preparation device and process flow of diisopropylbenzene hydroperoxide. According to the process, 1, 4-diisopropyl is taken as a raw material, and the diisopropylbenzene hydroperoxide is prepared through raw material pretreatment, oxidation, gas-liquid separation, concentration and filtration. According to the preparation process of the diisopropylbenzene hydroperoxide provided by the invention, concentration is performed twice, so that the concentration of the product is greatly improved. The unreacted raw material diisopropylbenzene returns to the raw material tank for recycling after being condensed, so that the raw material utilization rate is improved, the production cost is reduced, and the method is suitable for industrial production. The recorded process flow is simple, the raw material recovery rate is high, and the method is green and environment-friendly.

Description

Technical Field

[0001] The invention belongs to the field of chemical product devices, and in particular relates to a diisopropylbenzene hydroperoxide device and a process flow. Background Art

[0002] Organic peroxides have one or more peroxide bonds. Under light or heating conditions, the peroxide bonds break, so they are used as free radical polymerization initiators. Diisopropylbenzene hydroperoxide (DIP), also known as 3,5-diisopropylbenzene hydroperoxide, is an organic peroxide with a structure shown in Formula I. DIP is mainly used as a polymerization oxidant (initiator) for styrene-butadiene rubber. The free radicals generated by decomposition in the reaction enter the solubilized monomer micelles to initiate the monomers to generate free radicals for polymerization. In addition, DIP can also be used as an initiator for other polymers such as polyethylene, polyvinyl chloride, and synthetic resins.

[0003]

[0004] The traditional production method of organic peroxides is acid-catalyzed synthesis, and the catalyst is mainly divided into two types: homogeneous catalysts and heterogeneous catalysts. Homogeneous catalysts usually use concentrated hydrochloric acid, nitric acid and phosphoric acid, and strong acids will inevitably corrode the equipment during the production process. In addition, the preparation of peroxides in the reaction process of homogeneous production is violent, there are potential safety hazards, and homogeneous catalysts are usually not reusable, and the post-processing cost is high. In the process of preparing organic peroxides in traditional intermittent reactor reactors, the reaction conditions in the reactor are complex, the process parameters are difficult to accurately control, there are many by-products, and the utilization rate of raw materials is low, which puts severe requirements on the design of the process flow and the operating conditions. Therefore, it is necessary to improve the existing process and improve the level of equipment automation, so as to reduce costs, improve product quality and output, to meet the various needs of domestic and foreign markets for diisopropylbenzene hydroperoxide and related products, and also to make the by-products in the production process effectively utilized to avoid causing environmental pollution. Summary of the invention

[0005] In view of the problems existing in the background technology, the present invention provides a device and a process flow for preparing diisopropylbenzene hydroperoxide, which has simple process flow, high raw material recovery rate, high degree of automation and is green and environmentally friendly.

[0006] In order to achieve the above-mentioned purpose of the present invention, the following technical scheme is adopted:

[0007] A first aspect of the present invention provides a diisopropylbenzene hydroperoxide preparation device, which includes a raw material pretreatment unit, an oxidation reaction unit, a concentration unit and a filtering configuration unit.

[0008] In the preferred embodiment, the raw material pretreatment unit includes a raw material tank TK-109A / B / C, an overflow tank V-303, and an oxidation feed tank TK-101A / B / C.

[0009] In a further preferred scheme, the oxidation reaction unit includes an oxidation tower T-101, an air buffer tank V-305B, an oxidation external circulation pump PU-108A / B, an external circulation preheater E-301, an air cooler K-101, an oxidation liquid gas-liquid separator TK-102, an oxidation liquid cooler SE-101, an oxidation liquid storage tank TK-103A / B, an oxidation tail gas condenser SE-401, an oxidation tail gas gas-liquid separator TK-112, and a tailings tank TK-113.

[0010] In a further preferred scheme, the concentration unit includes a concentration feed pump PU-102A / B, a rising film evaporator SE-102 / SE-104, a flash tower T-102 / T-103, a concentration condenser E-501 / E-502, a concentration top liquid intermediate tank TK-108, a special concentration top liquid pump PU-106, a concentration cooler SE-193 / SE-105, a primary concentration storage tank TK-111, a concentrate liquid storage tank TK-105, a semi-finished product pump PU-105, and a semi-finished product storage tank TK-107A / B / C / D / E / F.

[0011] In a further preferred embodiment, the filtering configuration unit includes a DIP feed pump PU-113, a filter stirring tank, a filter V-315A / B, and a stirring kettle TK-106 / TK114.

[0012] The second aspect of the present invention provides a process for preparing diisopropylbenzene hydroperoxide, which comprises the following steps:

[0013]

[0014] Step 1: The raw material diisopropylbenzene is washed with caustic soda solution and then enters the oxidation tower.

[0015] Step 2: After entering the oxidation tower, the temperature is raised for oxidation. When the oxidized liquid reaches a certain concentration, the gas and liquid are separated and the liquid is cooled and stored.

[0016] Step 3: The material is flash-distilled and separated. The light component (diisopropylbenzene) is condensed and then enters the diisopropylbenzene raw material tank TK-109A / B / C for recycling. The heavy component is secondary concentrated and enters the semi-finished product storage tank.

[0017] TK-107A / B / C / D / E / F.

[0018] Step 4: After the semi-finished product storage tank TK-107 material reaches a certain concentration, the semi-finished product storage tank material passes through the DIP feed pump PU-113, and the diisopropylbenzene hydroperoxide material is mixed with the diatomaceous earth filter agent and filtered, and then the concentration is adjusted to prepare the finished product diisopropylbenzene hydroperoxide. The final configured product diisopropylbenzene hydroperoxide is filled after secondary filtration.

[0019] In a further preferred embodiment, the concentration of the alkali solution in Step 1 is 10-15%.

[0020] In the preferred embodiment, the alkali solution in Step 1 is prepared by using the external alkali to prepare a 10-15% caustic soda solution through the concentrated alkali tank V-302, and the prepared 10-15% caustic soda solution is pumped into the alkali washing tower T-301, and the alkali solution flows out from the bottom of the alkali washing tower T-301 for recycling.

[0021] In the preferred scheme, the pretreatment process of diisopropylbenzene in the device in Step 1 is that the raw material diisopropylbenzene delivered by the tank truck is unloaded into the diisopropylbenzene raw material tank TK-109A / B / C by the unloading pump. The diisopropylbenzene in the raw material tank TK-109 is sent out by P-304A / B. First, it enters the alkali washing tower T-301 from the bottom. There is a 10-15% caustic soda solution in the alkali washing tower T-301. The diisopropylbenzene washed from the top of the alkali washing tower enters the overflow tank V-303, overflows to the oxidation feed tank TK-101A / B / C, and then is sent to the oxidation tower T-101 for oxidation through the oxidation feed pump PU-101A / B.

[0022] In the preferred scheme, the oxidation step in Step 2 is that when the liquid level of the oxidation tower T-101 reaches 40%, air is introduced into the oxidation tower through the air buffer tank V-305B, and the oxidation external circulation pump PU-108A / B is turned on to start the material circulation of the oxidation tower T-101; the oxidation tower material begins to oxidize, and when the concentration of the oxidizing liquid in the tower reaches a certain concentration, the oxidation tower discharge valve is opened to separate the gas and liquid and store the liquid after cooling.

[0023] In a further preferred embodiment, the conditions in the oxidation tower are a temperature of about 80° C. and a pressure of about 0.30 MPa.

[0024] In a further preferred embodiment, when the concentration of the oxidation liquid in the tower reaches ≥15%, the discharge valve of the oxidation tower is opened.

[0025] In the preferred scheme, the liquid storage step after gas-liquid separation and cooling is that the oxidizing liquid enters the oxidizing liquid gas-liquid separator TK-102 through the air cooler K-101, and then enters the oxidizing liquid cooler SE-101 after gas-liquid separation, and enters the oxidizing liquid storage tank TK-103A / B after cooling.

[0026] In the preferred scheme, the oxidation reaction process inevitably produces waste gas. During the oxidation process, the tail gas from the top of the oxidation tower T-101 enters the oxidation tail gas condenser SE-401 for condensation, and then enters the oxidation tail gas gas-liquid separator TK-112 for gas-liquid separation. The condensate enters the tail material tank TK-113, and the non-condensable tail gas is discharged through tail gas treatment.

[0027] In a further preferred embodiment, the concentration unit in Sept 3 is operated under vacuum.

[0028] In the preferred scheme, the conditions for flash separation in Sept 3 are as follows: the flash tower pressure is first adjusted to about -0.098 MPa by a vacuum pump, and then the material in the oxidation liquid storage tank TK-103A / B is passed through the concentration feed pump PU-102A / B and enters the flash tower T-102 / T-103 through the rising film evaporator SE-102 / SE-104 and heated to about 120°C, and then enters the flash tower T-102 / T-103, and flash separation is carried out in the flash tower.

[0029] In the preferred scheme, the process of the reflux diisopropylbenzene of the light component raw material diisopropylbenzene in Sept 3 is that the light component (diisopropylbenzene) is condensed by the concentration condenser E-501 / E-502, and the condensate enters the concentration top liquid intermediate tank TK-108, and then the material is pumped back to the diisopropylbenzene raw material tank TK-109A / B / C for recycling through the concentration top liquid pump PU-106.

[0030] In the preferred embodiment, the material concentration of the semi-finished product storage tank TK-107 in Sept 4 is ≥58% of diisopropylbenzene hydroperoxide, and the material from the semi-finished product storage tank passes through the DIP feed pump PU-113.

[0031] In a further preferred embodiment, the concentration of the finished product diisopropylbenzene hydroperoxide in Sept 4 is 54.5±0.5%.

[0032] The diisopropylbenzene hydroperoxide preparation device and process provided by the present invention have the following advantages:

[0033] (1) The unreacted raw material diisopropylbenzene in the process for preparing diisopropylbenzene hydroperoxide provided by the present invention is condensed and then returned to the raw material tank for recycling, thereby improving the utilization rate of raw materials, greatly reducing costs, and being suitable for industrial production.

[0034] (2) The process for preparing diisopropylbenzene hydroperoxide provided in the present invention undergoes two concentration steps, thereby increasing the concentration of the product.

[0035] (3) The present invention adopts diatomaceous earth filtration, which has a porous structure, a large surface area, and a high porosity. It is flexible, safe, effective, and low-cost as a filter.

[0036] (4) The process route designed in this patent is excellent. Workers do not need to participate in the transfer of materials, and the materials are prevented from being contaminated by exposure to the air. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 Schematic diagram of the process flow for preparing diisopropylbenzene hydroperoxide DETAILED DESCRIPTION

[0038] The following embodiments of the technical solution of the present invention are described in detail in conjunction with the embodiments. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and are therefore only used as examples, and cannot be used to limit the protection scope of the present invention.

[0039] It should be noted that the experimental methods used in the implementation examples are all conventional methods unless otherwise specified; the materials, reagents, etc. used, unless otherwise specified, can be obtained from commercial channels.

[0040] In the present invention, unless otherwise specified, the numerical range "a-b" represents an abbreviation of any real number combination between a-b, where a and b are real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" are listed in this document, and "0-5" is just an abbreviation of these numerical combinations.

[0041] In the present invention, unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined with each other to form a new technical solution.

[0042] In the present invention, unless otherwise specified, all the steps mentioned herein may be performed sequentially or randomly, but are preferably performed sequentially; for example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially; for example, the method may further include step (c), which means that step (c) may be added to the method in any order, for example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0043] In the present invention, unless otherwise specified, the specific numerical values ​​and specific substances in the embodiments of the present invention may be combined with other features of the description part of the present invention; for example, if the specification mentions that the reaction temperature is 10-100°C, and the embodiment mentions that the reaction temperature is 20°C, then it can be considered that the present invention has specifically disclosed the range of 10-20°C, or the range of 20-100°C, and this range can be combined with other features of the description part to form a new technical solution.

[0044] The preferred solution is Figure 1 As shown, the present invention is a process for preparing diisopropylbenzene hydroperoxide, and the steps are as follows:

[0045] Step 1: The raw material diisopropylbenzene is washed with caustic soda solution and then enters the oxidation tower.

[0046] Step 2: After entering the oxidation tower, the temperature is raised for oxidation. When the oxidized liquid reaches a certain concentration, the gas and liquid are separated and the liquid is cooled and stored.

[0047] Step 3: The material is flash-distilled and separated. The light component (diisopropylbenzene) is condensed and then enters the diisopropylbenzene raw material tank TK-109A / B / C for recycling. The heavy component is secondary concentrated and enters the semi-finished product storage tank.

[0048] TK-107A / B / C / D / E / F.

[0049] Step 4: After the semi-finished product storage tank TK-107 material reaches a certain concentration, the semi-finished product storage tank material passes through the DIP feed pump PU-113, and the diisopropylbenzene hydroperoxide material is mixed with the diatomaceous earth filter agent and filtered, and then the concentration is adjusted to prepare the finished product diisopropylbenzene hydroperoxide. The final configured product diisopropylbenzene hydroperoxide is filled after secondary filtration.

[0050] Example 1

[0051] (1) Alkali solution preparation: The external alkali is prepared into 10-15% caustic soda solution through the concentrated alkali tank V-302, and the prepared 10-15% caustic soda solution is pumped into the alkali washing tower T-301. The alkali solution flows out from the bottom of the alkali washing tower T-301 for recycling.

[0052] (2) Raw material pretreatment: The raw material diisopropylbenzene is delivered by a tank truck and unloaded into the diisopropylbenzene raw material tank TK-109A / B / C by a truck unloading pump. The diisopropylbenzene in the raw material tank TK-109 is sent out by P-304A / B. First, it enters the alkali washing tower T-301 from the bottom. There is a prepared 10-15% caustic soda solution in the alkali washing tower T-301. The diisopropylbenzene washed from the top of the alkali washing tower enters the overflow tank V-303, overflows to the oxidation feed tank TK-101A / B / C, and then is sent to the oxidation tower T-101 for oxidation through the oxidation feed pump PU-101A / B.

[0053] (3) Oxidation: When the liquid level of oxidation tower T-101 reaches 40%, air is introduced into the oxidation tower through air buffer tank V-305B, and oxidation external circulation pump PU-108A / B is turned on to start the circulation of materials in oxidation tower T-101. The temperature in the tower is adjusted to about 80°C through external circulation preheater E-301, and the pressure is adjusted to about 0.30 MPa; the oxidation tower material begins to oxidize.

[0054] (4) Gas-liquid separation: When the concentration of the oxidizing liquid in the tower reaches ≥15%, the discharge valve of the oxidation tower is opened, and the oxidizing liquid enters the oxidizing liquid gas-liquid separator TK-102 through the air cooler K-101. After gas-liquid separation, it enters the oxidizing liquid cooler SE-101 and enters the oxidizing liquid storage tank TK-103A / B after cooling.

[0055] (5) Oxidation tower tail gas treatment: The tail gas from the top of the oxidation tower T-101 enters the oxidation tail gas condenser SE-401 for condensation, and then enters the oxidation tail gas gas-liquid separator TK-112 for gas-liquid separation. The condensate enters the tail material tank TK-113, and the non-condensable tail gas is discharged through tail gas treatment.

[0056] (6) Concentration: The concentration unit is vacuum operated. The flash tower is first adjusted to a pressure of about -0.098 MPa by a vacuum pump. The material in the oxidation liquid storage tank TK-103A / B is then fed into the flash tower T-102 / T-103 through the concentration feed pump PU-102A / B and heated to about 120°C by the rising film evaporator SE-102 / SE-104. The material is then flashed and separated in the flash tower. The light component (diisopropylbenzene) is condensed by the concentration condenser E-501 / E-502 and the condensate enters the concentration top liquid. In the intermediate tank TK-108, the material is pumped back to the diisopropyl raw material tank TK-109A / B / C for recycling through the top liquid pump PU-106. The heavy component diisopropylbenzene hydroperoxide is cooled by the concentration cooler SE-103 / SE-105 and then enters the primary concentration storage tank TK-111. It is then concentrated for the second time through the flash tower. The concentrated liquid after the second concentration enters the concentrated liquid storage tank TK-105 and is then pumped into the semi-finished product storage tank TK-107A / B / C / D / E / F through the semi-finished product pump PU-105.

[0057] (7) Filtration: The material concentration of the semi-finished product storage tank TK-107 is ≥58% of diisopropylbenzene hydroperoxide. The material from the semi-finished product storage tank is pumped into the filter stirring tank through the DIP pump PU-113, mixed with the diatomaceous earth filter agent, and then pumped into the filter V-315A / B for filtration.

[0058] (8) Preparation: The filtered diisopropylbenzene hydroperoxide enters the stirred tank TK-106 / TK114 for preparation, and the concentration of the finished diisopropylbenzene hydroperoxide needs to be adjusted to 54.5±0.5%. The final prepared product diisopropylbenzene hydroperoxide is filled after secondary filtration.

Claims

1. A device and process flow for preparing diisopropylbenzene hydroperoxide, comprising a raw material pretreatment unit, an oxidation reaction unit, a concentration unit and a filtration configuration unit. The raw material pretreatment unit includes raw material tank TK-109A / B / C, overflow tank V-303, and oxidation feed tank TK-101A / B / C. The oxidation reaction unit includes oxidation tower T-101, air buffer tank V-305B, oxidation external circulation pump PU-108A / B, external circulation preheater E-301, air cooler K-101, oxidation liquid gas-liquid separator TK-102, oxidation liquid cooler SE-101, oxidation liquid storage tank TK-103A / B, oxidation tail gas condenser SE-401, oxidation tail gas gas-liquid separator TK-112, and tailings tank TK-113. The concentration unit includes concentration feed pump PU-102A / B, rising film evaporator SE-102 / SE-104, flash tower T-102 / T-103, concentration condenser E-501 / E-502, concentration top liquid intermediate tank TK-108, special concentration top liquid pump PU-106, concentration cooler SE-193 / SE-105, primary concentration storage tank TK-111, concentrate liquid storage tank TK-105, semi-finished product pump PU-105, and semi-finished product storage tank TK-107A / B / C / D / E / F. The filtration configuration unit includes DIP feed pump PU-113, filter stirring tank, filter V-315A / B, and stirring kettle TK-106 / TK114.

2. The diisopropylbenzene hydroperoxide preparation device according to claim 1, characterized in that: The process flow of preparing diisopropylbenzene hydroperoxide is as follows: Step 1: The raw material diisopropylbenzene is washed with 10-15% caustic soda solution and then enters the oxidation tower. Step 2: After entering the oxidation tower, the temperature is raised for oxidation. When the oxidized liquid reaches a certain concentration, the gas and liquid are separated and the liquid is cooled and stored. Step 3: The material is flash-separated, the light component (diisopropylbenzene) is condensed and enters the diisopropylbenzene raw material tank TK-109A / B / C for recycling, and the heavy component is secondary concentrated and enters the semi-finished product storage tank TK-107A / B / C / D / E / F. The concentration unit is vacuum operated. Step 4: The semi-finished product storage tank TK-107 material concentration is ≥58% of diisopropylbenzene hydroperoxide. After the semi-finished product storage tank material passes through the DIP material pump PU-113 to a certain concentration, the semi-finished product storage tank material passes through the DIP material pump PU-113, the diisopropylbenzene hydroperoxide material is mixed with the diatomaceous earth filter agent and filtered, and then the concentration is adjusted to prepare the finished product diisopropylbenzene hydroperoxide. The final configured product diisopropylbenzene hydroperoxide is filled after secondary filtration.

3. The process for preparing diisopropylbenzene hydroperoxide according to claim 2, characterized in that: In Step 1, the alkali solution is prepared by adding external alkali to a 10-15% caustic soda solution through a concentrated alkali tank V-302, and the prepared 10-15% caustic soda solution is pumped into an alkali washing tower T-301, and the alkali solution flows out from the bottom of the alkali washing tower T-301 for recycling.

4. The process for preparing diisopropylbenzene hydroperoxide according to claim 2, characterized in that: In Step 1, the pretreatment process of diisopropylbenzene in the device is that the raw material diisopropylbenzene delivered by the tank truck is unloaded into the diisopropylbenzene raw material tank TK-109A / B / C by the unloading pump. The diisopropylbenzene in the raw material tank TK-109 is sent out by P-304A / B. First, it enters the alkali washing tower T-301 from the bottom. There is a prepared 10-15% caustic soda solution in the alkali washing tower T-301. The diisopropylbenzene washed from the top of the alkali washing tower enters the overflow tank V-303, overflows to the oxidation feed tank TK-101A / B / C, and then is sent to the oxidation tower T-101 for oxidation through the oxidation feed pump PU-101A / B.

5. The process of diisopropylbenzene hydroperoxide according to claim 2, characterized in that: In Step 2, when the liquid level of oxidation tower T-101 reaches 40%, air is introduced into the oxidation tower through air buffer tank V-305B, and oxidation external circulation pump PU-108A / B is turned on to start the material circulation of oxidation tower T-101; the temperature in the oxidation tower is about 80°C and the pressure is about 0.30mpa. The oxidation tower material begins to oxidize, and when the concentration of the oxidation liquid in the tower is ≥15%, the oxidation tower discharge valve is opened to separate the gas and liquid and store the liquid after cooling.

6. The oxidation step according to claim 5, characterized in that The liquid storage step after gas-liquid separation and cooling is that the oxidizing liquid enters the oxidizing liquid gas-liquid separator TK-102 through the air cooler K-101, and then enters the oxidizing liquid cooler SE-101 after gas-liquid separation, and enters the oxidizing liquid storage tank TK-103A / B after cooling.

7. The Step 2 oxidation reaction unit according to claim 2, characterized in that: The oxidation reaction process inevitably produces waste gas. During the oxidation process, the tail gas from the top of the oxidation tower T-101 enters the oxidation tail gas condenser SE-401 for condensation, and then enters the oxidation tail gas gas-liquid separator TK-112 for gas-liquid separation. The condensate enters the tail material tank TK-113, and the non-condensable tail gas is discharged through tail gas treatment.

8. The process for preparing diisopropylbenzene hydroperoxide according to claim 2, characterized in that: The flash separation condition in Sept 3 is that the flash tower pressure is first adjusted to about -0.098 MPa by a vacuum pump, and then the material in the oxidation liquid storage tank TK-103A / B is fed into the flash tower T-102 / T-103 through the concentration feed pump PU-102A / B, heated to about 120°C by the rising film evaporator SE-102 / SE-104, and then enters the flash tower T-102 / T-103 for flash separation.

9. The process for preparing diisopropylbenzene hydroperoxide according to claim 2, characterized in that: The process of the reflux diisopropylbenzene raw material tank TK-109A / B / C of the light component raw material in Sept 3 is as follows: after the light component (diisopropylbenzene) is condensed by the concentration condenser E-501 / E-502, the condensate enters the concentration top liquid intermediate tank TK-108, and then the material is pumped back to the diisopropylbenzene raw material tank TK-109A / B / C for recycling through the concentration top liquid pump PU-106.

10. The process for preparing diisopropylbenzene hydroperoxide according to claim 2, characterized in that: The concentration of the finished diisopropylbenzene hydroperoxide in Sept 4 was 54.5 ± 0.5%.

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