A continuous production system and method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane

Abstract

The present application relates to the technical field of chemical production, in particular to a continuous production system and method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane, comprising a 2,5-dimethyl-2,5-hexanediol storage tank and a tert-butyl hydroperoxide storage tank, both of which are connected to the feeding end of a dynamic tubular reactor, the discharging end of the dynamic tubular reactor is connected to a buffer tank, the discharging end of the buffer tank is connected to a micro-channel reactor, the feeding end of the micro-channel reactor is also connected to a sulfuric acid storage tank, and the discharging end of the micro-channel reactor is sequentially connected to a reaction kettle, a time-delay reactor and a product storage tank. The present application combines the peroxidation reaction and tert-butylation reaction into one step, avoids the complex operation of the traditional two-step method, can realize the continuous production of the factory, avoids the additional manpower and material resources consumed by the intermittent production start and stop, and reduces the energy consumption.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical production, in particular to a continuous production system and method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane. BACKGROUND

[0002] 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane is an important organic peroxide, mainly used as a vulcanizing agent for silicone rubber and a chemical modifier for polypropylene. The traditional synthesis of the bifunctional organic peroxide 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane is carried out by two-step method of peroxidation and tert-butylation. The peroxidation reaction is to synthesize 2,5-dimethyl-2,5-bis(peroxy)hexane by oxidation reaction with 2,5-dimethyl-2,5-hexanediol and hydrogen peroxide as raw materials under the catalysis of sulfuric acid; the tert-butylation reaction is completed by 2,5-dimethyl-2,5-bis(peroxy)hexane and tert-butyl alcohol. The existing production system is intermittent, and the peroxidation and tert-butylation raw materials are all solids which need to be dissolved before the next reaction, so the production cannot be continuous, the efficiency is low, and a large amount of manpower is wasted.

[0003] Chinese patent (CN101880254A) discloses a preparation method of 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, which includes peroxidation reaction and tert-butylation reaction. The sulfuric acid added in the peroxidation reaction is 70-85%, the reaction temperature is 20-48℃, and the reaction time is 30-60 minutes; sulfuric acid and hydrogen peroxide are added in the filtrate to reach the proportion of peroxidation reaction raw materials, and 2,5-dimethyl-2,5-hexanediol is added as new peroxidation reaction raw materials. In the inorganic phase after tert-butylation reaction, tert-butyl alcohol and sulfuric acid are added to reach the proportion of tert-butylation reaction raw materials of tert-butyl alcohol and sulfuric acid, and 2,5-dimethyl-2,5-bis(peroxy)hexane is added as new tert-butylation reaction raw materials. Although this invention method can obtain high-concentration product, the process is complex and the raw materials of each step are solids, which is difficult to carry out industrial continuous production. Therefore, it is urgent to develop a new continuous production process of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane to solve the deficiencies in the existing production method, realize the continuous production of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane, and improve the production efficiency of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane. SUMMARY

[0004] To solve the problems in the prior art, the present application provides a continuous production system and method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane.

[0005] In order to achieve the above-mentioned purpose, the technical scheme of the present application is as follows: a continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane, comprising a 2,5-dimethyl-2,5-hexanediol storage tank and a tert-butyl peroxide storage tank, the 2,5-dimethyl-2,5-hexanediol storage tank and the tert-butyl peroxide storage tank are both connected to the feeding end of a dynamic tubular reactor, the discharging end of the dynamic tubular reactor is connected with a buffer tank, the discharging end of the buffer tank is connected with a micro-channel reactor, the feeding end of the micro-channel reactor is also connected with a sulfuric acid storage tank, and the discharging end of the micro-channel reactor is sequentially connected with a reaction kettle, a delay reactor and a product storage tank.

[0006] Further, a spiral feeding device is arranged between the 2,5-dimethyl-2,5-hexanediol storage tank and the dynamic tubular reactor.

[0007] Further, a pump A is arranged between the tert-butyl peroxide storage tank and the dynamic tubular reactor, a pump B is arranged between the buffer tank and the micro-channel reactor, a pump C is arranged between the sulfuric acid storage tank and the micro-channel reactor, and a pump D is arranged between the reaction kettle and the delay reactor.

[0008] Further, the pump A, the pump B, the pump C and the pump D are all plunger pumps.

[0009] Further, a cooling medium inlet A and a cooling medium outlet A are arranged on the dynamic tubular reactor.

[0010] Further, a cooling medium inlet B and a cooling medium outlet B are arranged on the micro-channel reactor.

[0011] Further, a heating medium inlet and a heating medium outlet are arranged on the reaction kettle.

[0012] Further, a stirring device is arranged in the 2,5-dimethyl-2,5-hexanediol storage tank.

[0013] A continuous production method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane, which is based on the continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane and works as follows:

[0014] (1) powder 2,5-dimethyl-2,5-hexanediol is added into the 2,5-dimethyl-2,5-hexanediol storage tank, tert-butyl alcohol peroxide is added into the tert-butyl peroxide storage tank, and then the 2,5-dimethyl-2,5-hexanediol and the tert-butyl alcohol peroxide are mixed in the dynamic tubular reactor and then enter the buffer tank;

[0015] (2) the mixed material of step (1) and sulfuric acid in the sulfuric acid storage tank are added into a micro-channel reactor for mixing, and after mixing, they are added into a reaction kettle for reaction, and the product after reaction is further reacted in a time-delay reactor and then added into a product storage tank.

[0016] Further, the molar ratio of 2,5-dimethyl-2,5-hexanediol, tert-butyl alcohol peroxide and sulfuric acid is 1:1.5-2.08:2.08, the mixing temperature in the dynamic tubular reactor is 20-30℃, the mixing temperature in the micro-channel reactor is 28-30℃, and the reaction temperature in the reaction kettle is 38-40℃.

[0017] The present application has the following beneficial effects:

[0018] 1. The present application combines the peroxidation reaction and the tert-butylation reaction into one step, avoids the complex operation of the traditional two-step method, can realize continuous production in a factory, avoids the additional manpower and material resources consumed by intermittent production start and stop, and reduces energy consumption.

[0019] 2. The present application reduces the amount of sulfuric acid used, reduces factory pollution, and meets the green chemistry concept.

[0020] 3. The present application uses tert-butyl peroxide to avoid using hydrogen peroxide, greatly reduces the risk of the reaction process, ensures the smooth and safe progress of the entire reaction, and at the same time, the present application uses tert-butyl peroxide to dissolve hexanediol, avoiding the operation mode of adding tert-butyl alcohol peroxide after dissolving hexanediol with sulfuric acid in the traditional method, greatly reducing the amount of cyclic by-products.

[0021] 4. The dynamic tubular reactor designed in the present application can realize the sufficient mixing of tert-butyl peroxide and 2,5-dimethyl-2,5-hexanediol, so that the reaction can be carried out more fully.

[0022] 5. The micro-channel reactor designed in the present application can dissipate heat in time, can greatly reduce the generation of cyclic by-products, and shorten the reaction time. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 is a schematic diagram of the overall structure of the present application.

[0024] Explanation of the marks in the figure: 1. 2,5-dimethyl-2,5-hexanediol storage tank; 2. Screw feeding device; 3. Dynamic tubular reactor; 4. Cooling medium inlet A; 5. Cooling medium outlet A; 6. Tert-butyl peroxide storage tank; 7. Pump A; 8. Buffer tank; 9. Pump B; 10. Microchannel reactor; 11. Cooling medium inlet B; 12. Cooling medium outlet B; 13. Sulfuric acid storage tank; 14. Pump C; 15. Reactor; 16. Heating medium inlet; 17. Heating medium outlet; 18. Pump D; 19. Delay reactor; 20. Product storage tank. DETAILED DESCRIPTION

[0025] In order to better understand the purpose, structure and function of the present invention, the following is a further detailed description of a continuous production system and method of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane of the present invention in conjunction with the accompanying drawings.

[0026] Example 1

[0027] like Figure 1 As shown, a continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane includes a mixing system and a reaction system connected to each other.

[0028] The mixing system includes a 2,5-dimethyl-2,5-hexanediol storage tank 1, a screw feeding device 2, a dynamic tubular reactor 3, a buffer tank 8, a microchannel reactor 10 and a sulfuric acid storage tank 13. A stirring device is provided inside the 2,5-dimethyl-2,5-hexanediol storage tank 1 to prevent the 2,5-dimethyl-2,5-hexanediol powder from piling up and sticking in the 2,5-dimethyl-2,5-hexanediol storage tank 1. The bottom discharge end of the 2,5-dimethyl-2,5-hexanediol storage tank 1 is connected to a screw feeding device 2. The other end of the screw feeding device 2 is connected to the bottom discharge end of the 2,5-dimethyl-2,5-hexanediol storage tank 1. One end is connected to the feed end of the dynamic tubular reactor 3, and the other feed end of the dynamic tubular reactor 3 is connected to the tert-butyl peroxide storage tank 6. A pump A7 is provided between the tert-butyl peroxide storage tank 6 and the dynamic tubular reactor 3. A cooling medium inlet A4 and a cooling medium outlet A5 are provided on the dynamic tubular reactor 3. The cooling medium inlet A4 and the cooling medium outlet A5 control the temperature in the dynamic tubular reactor 3 to be the optimal temperature for mixing. The dynamic tubular reactor 3 can fully mix and dissolve 2,5-dimethyl-2,5-hexanediol and tert-butyl peroxide.

[0029] The dynamic tubular reactor 3 is connected with a buffer tank 8 at the discharge end, the buffer tank 8 is connected with a micro-channel reactor 10 at the discharge end through a pump B9, the micro-channel reactor 10 is connected with a sulfuric acid storage tank 13 at the other feeding end, the micro-channel reactor 10 is provided with a cooling medium inlet B11 and a cooling medium outlet B12, and the micro-channel reactor 10 further mixes 2,5-dimethyl-2,5-hexanediol, t-butyl peroxide and sulfuric acid.

[0030] The reaction system comprises a reaction kettle 15 connected with the micro-channel reactor 10 at the discharge end, the reaction kettle 15 is provided with a heating medium inlet 16 and a heating medium outlet 17, and the reaction kettle 15 is connected with a delay reactor 19 at the discharge end through a pump D18, and the delay reactor 19 is connected with a product storage tank 20 at the discharge end.

[0031] Among them, the pump A7, the pump B9, the pump C14 and the pump D18 are all plunger pumps.

[0032] A continuous production method of 2,5-dimethyl-2,5-bis-(t-butyl peroxy) hexane, and the reaction formula is as follows:

[0033]

[0034] The method comprises the following steps:

[0035] (1) Mixing process

[0036] The powder 2,5-dimethyl-2,5-hexanediol is added into the 2,5-dimethyl-2,5-hexanediol storage tank 1, the t-butyl alcohol peroxide is added into the t-butyl peroxide storage tank 6, the molar ratio of 2,5-dimethyl-2,5-hexanediol to t-butyl alcohol peroxide is 1:1.5-2.08, the powder 2,5-dimethyl-2,5-hexanediol enters the dynamic tubular reactor 3 through the screw feeding device 2, the t-butyl peroxide enters the dynamic tubular reactor 3 through the pump A7, the 2,5-dimethyl-2,5-hexanediol and the t-butyl alcohol peroxide are mixed and dissolved in the dynamic tubular reactor 3, the mixing temperature in the dynamic tubular reactor 3 is 20-30℃, and the mixed 2,5-dimethyl-2,5-hexanediol and t-butyl alcohol peroxide enter the buffer tank 8 for storage. The 2,5-dimethyl-2,5-hexanediol and t-butyl alcohol peroxide mixture in the buffer tank 8 is mixed with sulfuric acid entering the micro-channel reactor 10 from the sulfuric acid storage tank 13, the mixing temperature in the micro-channel reactor 10 is 28-30℃, and the molar ratio of 2,5-dimethyl-2,5-hexanediol, t-butyl alcohol peroxide and sulfuric acid is 1:1.5-2.08:2.08.

[0037] (2) Reaction process

[0038] The mixed solution is introduced into the reactor 15 for stirring reaction, the reaction temperature in the reactor 15 is 38-40℃, the reaction time is 2h, and the reaction product is introduced into the product storage tank 20 after further reaction in the time-delay reactor 19.

[0039] Example 2

[0040] The 2,5-dimethyl-2,5-hexanediol powder is introduced into the dynamic tubular reactor 3 through the screw feeding device 2 at a flow rate of 14.6g / min, while the tertiary butyl hydroperoxide with a mass fraction of 80% is introduced into the dynamic tubular reactor 3 through the plunger pump A7 at a flow rate of 23.4g / min, the mixing temperature is 25℃, the mixing time is 5min, and the mixed 2,5-dimethyl-2,5-hexanediol and tertiary butyl hydroperoxide mixture is stored in the buffer tank 8.

[0041] The mixed 2,5-dimethyl-2,5-hexanediol and tertiary butyl hydroperoxide is introduced into the micro-channel reactor 10 through the plunger pump B9 at a flow rate of 38g / min, the sulfuric acid with a mass fraction of 75% is introduced into the micro-channel reactor 10 through the plunger pump C14 at a flow rate of 27.2g / min, the molar ratio of 2,5-dimethyl-2,5-hexanediol, tertiary butyl hydroperoxide and sulfuric acid is 1:2.08:2.08, the 2,5-dimethyl-2,5-hexanediol, tertiary butyl hydroperoxide and sulfuric acid are mixed in the micro-channel reactor 10, the mixing temperature is 28℃, and the residence time of the micro-channel reactor 10 is 3min.

[0042] The mixed 2,5-dimethyl-2,5-hexanediol, tertiary butyl hydroperoxide and sulfuric acid is introduced into the reactor 15 for stirring reaction, the reaction temperature is 40℃, and the reaction time is 2h. After the reaction is completed, the phases are separated, the upper organic phase is taken for alkali washing, the upper organic phase after alkali washing is taken, and the yield of the crude 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane is 62.1% through calculation.

[0043] Example 3

[0044] The 2,5-dimethyl-2,5-hexanediol powder is introduced into the dynamic tubular reactor 3 through the screw feeding device 2 at a flow rate of 14.6g / min, while the tertiary butyl hydroperoxide with a mass fraction of 80% is introduced into the dynamic tubular reactor 3 through the plunger pump A7 at a flow rate of 23.4g / min, the mixing temperature is 25℃, the mixing time is 5min, and the mixed 2,5-dimethyl-2,5-hexanediol and tertiary butyl hydroperoxide mixture is stored in the buffer tank 8.

[0045] The mixed 2,5-dimethyl-2,5-hexanediol and tert-butyl hydroperoxide was fed into the micro-channel reactor 10 at a flow rate of 31.5 g / min by the plunger pump B9, the mass fraction 75% sulfuric acid was fed into the micro-channel reactor 10 at a flow rate of 27.2 g / min by the plunger pump C14, the molar ratio of 2,5-dimethyl-2,5-hexanediol, tert-butyl hydroperoxide and sulfuric acid was 1:1.5:2.08, the mixed 2,5-dimethyl-2,5-hexanediol, tert-butyl hydroperoxide and sulfuric acid was mixed in the micro-channel reactor 10, the mixing temperature was 28℃, and the residence time of the micro-channel reactor 10 was 3 min.

[0046] The mixed 2,5-dimethyl-2,5-hexanediol, tert-butyl hydroperoxide and sulfuric acid was fed into the reaction kettle 15 for stirring reaction, the reaction temperature was 40℃, and the reaction time was 2 h. After the reaction was completed, the phases were separated, the upper organic phase was taken for alkali washing, the upper organic phase after alkali washing was taken, and the yield of the crude 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane was 57.0% by calculation.

[0047] Comparative Example 1

[0048] The 36.5 g 2,5-dimethyl-2,5-hexanediol powder was fed into a glass kettle containing 58.5 g tert-butyl hydroperoxide with a mass fraction of 80%, the temperature in the kettle was controlled at 25℃, after the 2,5-dimethyl-2,5-hexanediol powder was completely dissolved, 68 g sulfuric acid with a mass fraction of 75% was added dropwise into the glass kettle, the temperature was controlled to be not more than 40℃, at this time, the molar ratio of 2,5-dimethyl-2,5-hexanediol, tert-butyl hydroperoxide and sulfuric acid in the glass kettle was 1:2.08:2.08, after the sulfuric acid was added dropwise, the temperature was increased, the temperature in the kettle was controlled at 40℃, and the reaction was kept for 2 h. After the reaction was completed, the phases were separated, the upper organic phase was taken for alkali washing, the upper organic phase after alkali washing was taken, and the yield of the crude 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane was 63.6% by calculation.

[0049] Comparative Example 1 is a batch operation process for preparing 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane in the laboratory, the molar ratio of the reactants is the same as that of Example 2, and the yield of the crude 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane is also within the allowable error range, thereby proving the feasibility of the industrial continuous production of 2,5-dimethyl-2,5-bis-(tert-butylperoxy) hexane.

[0050] It is to be understood that the present application is described by way of example only, and that modifications or alterations can be made to the features and embodiments described without departing from the spirit and scope of the application. In addition, modifications can be made to the features and embodiments described to accommodate specific situations and materials without departing from the spirit and scope of the application. Accordingly, the application is not limited to the specific embodiments disclosed herein, but rather, the scope of the application includes all embodiments falling within the scope of the claims.

Claims

1. A continuous production system for 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane, characterized in that: The invention comprises a 2,5-dimethyl-2,5-hexanediol storage tank (1) and a tert-butyl peroxide storage tank (6), wherein the 2,5-dimethyl-2,5-hexanediol storage tank (1) and the tert-butyl peroxide storage tank (6) are both connected to the feed end of a dynamic tubular reactor (3), the discharge end of the dynamic tubular reactor (3) is connected to a buffer tank (8), the discharge end of the buffer tank (8) is connected to a microchannel reactor (10), and the feed end of the microchannel reactor (10) is also connected to a sulfuric acid storage tank ( 13), the discharge end of the microchannel reactor (10) is sequentially connected to a reactor (15), a time-delay reactor (19) and a product storage tank (20); the dynamic tubular reactor (3) is provided with a cooling medium inlet A (4) and a cooling medium outlet A (5), the microchannel reactor (10) is provided with a cooling medium inlet B (11) and a cooling medium outlet B (12), and the reactor (15) is provided with a heating medium inlet (16) and a heating medium outlet (17).

2. A continuous production system for 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to claim 1, characterized in that: A screw feeding device (2) is provided between the 2,5-dimethyl-2,5-hexanediol storage tank (1) and the dynamic tubular reactor (3).

3. A continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to claim 2, characterized in that: A pump A (7) is provided between the tert-butyl peroxide storage tank (6) and the dynamic tubular reactor (3), a pump B (9) is provided between the buffer tank (8) and the microchannel reactor (10), a pump C (14) is provided between the sulfuric acid storage tank (13) and the microchannel reactor (10), and a pump D (18) is provided between the reactor (15) and the time-delay reactor (19).

4. A continuous production system for 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to claim 3, characterized in that: The pump A (7), pump B (9), pump C (14) and pump D (18) are all plunger pumps.

5. A continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to claim 1, characterized in that: The 2,5-dimethyl-2,5-hexanediol storage tank (1) is provided with a stirring device.

6. A method for continuous production of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane, operating based on the continuous production system of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to any one of claims 1 to 5, characterized in that: The steps include: (1) Powdered 2,5-dimethyl-2,5-hexanediol is added to a 2,5-dimethyl-2,5-hexanediol storage tank (1), and tert-butyl peroxide is added to a tert-butyl peroxide storage tank (6). After the 2,5-dimethyl-2,5-hexanediol and tert-butyl peroxide are mixed in a dynamic tubular reactor (3), the mixture is then introduced into a buffer tank (8); (2) The mixed material in step (1) and the sulfuric acid in the sulfuric acid storage tank (13) are added to the microchannel reactor (10) for mixing. After mixing, the mixture enters the reactor (15) for reaction. The product after the reaction is further reacted in the delayed reactor (19) and then enters the product storage tank (20).

7. The method for continuous production of 2,5-dimethyl-2,5-bis-(tert-butylperoxy)hexane according to claim 6, characterized in that: The molar ratio of the 2,5-dimethyl-2,5-hexanediol, tert-butyl peroxide and sulfuric acid is 1:1.5-2.08:2.08, the mixing temperature in the dynamic tubular reactor (3) is 20-30°C, the mixing temperature in the microchannel reactor (10) is 28-30°C, and the reaction temperature in the reactor (15) is 38-40°C.

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