CN104592080A - Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow - Google Patents
Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow Download PDFInfo
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Abstract
The invention provides a method for preparing tert-butyl peroxyneodecanoate (BNP) through a continuous flow, wherein the method includes an alkaline aqueous solution is prepared, the alkaline aqueous solution and a tert-butyl hydrogen peroxide aqueous solution are subjected to a reaction in a reactor, a neodecanoyl chloride solution and the product of the alkaline aqueous solution and the tert-butyl hydrogen peroxide aqueous solution are subjected to a reaction, and the product is subjected to further full reaction through a delay pipeline to obtain the product, wherein the reaction process is carried out in a micro-reactor. With adopting of the prepared solvent-type or emulsion-type tert-butyl peroxyneodecanoate (BNP), the product quality is stable, and the reproducibility is good; because the reaction is carried out in the micro-reactor, the process flow is simplified, the reaction is continuously carried out under mild, safe and environmental-protection conditions, the amount and the yield of the product are greatly improved, and the yield can reach above 98%.
Description
Technical field
The present invention relates to the preparation method of the initiator type tert-butyl peroxyneo-caprate (BNP) of a kind of superpolymer synthesis, particularly a kind of Continuous Flow prepares the method for type tert-butyl peroxyneo-caprate (BNP), belongs to chemical field.
Background technology
Microreactor, i.e. micro passage reaction, the microreactor of the characteristic dimension utilizing precision processing technology to manufacture between 10 to 300 microns.Microreactor can make the passage of reacting fluid in micron level, millions of minitype channel can be included, simultaneously because the microstructure of its inside makes microreactor equipment have great specific surface area, the hundred times even thousands of times of stirring tank specific surface area can be reached.Microreactor has fabulous heat transfer and mass transfer ability, and the moment Homogeneous phase mixing that can realize material conducts heat with efficient, and therefore many reactions that cannot realize in conventional reactor can realize in microreactor.
Organo-peroxide is the organic compound after one or two hydrogen atom in hydrogen peroxide is substituted, and is mainly used in radical polymerization initiator, curable unsaturated polyester initiator, macromolecule crosslink agent, organic synthesis oxygenant, SYNTHETIC OPTICAL WHITNER and sterilant etc.Type tert-butyl peroxyneo-caprate (BNP) is as a kind of Macroscopic single crystal higher effective initiator, compared with common azo-initiator, in vinylchlorid, vinylbenzene, methacrylic ester and Polymerization of Vac process, consumption is few, efficiency of initiation is high, polyreaction heat release is even, and product performance are excellent.Meanwhile, type tert-butyl peroxyneo-caprate (BNP) is the high-temperature curing agent of the excellent low temperature initiators of high-pressure polyethylene and unsaturated polyester.
Industrialization type tert-butyl peroxyneo-caprate (BNP) is produced and is adopted andnon-continuous operation manner, and labor strength is large, and processing condition are affected by human factors comparatively large, quality stability and poor reproducibility.Meanwhile, due to the scantlings of the structure that reactor device interior is larger, the concentration of material in reaction process, temperature distributing disproportionation is even, causes type tert-butyl peroxyneo-caprate (BNP) finished activated hypoxgia, reduces product quality.
Summary of the invention
For prior art Problems existing, the invention provides a kind of method that Continuous Flow prepares type tert-butyl peroxyneo-caprate (BNP), adopt the mode of Continuous Flow to improve constant product quality and circulation ratio, reduce labor strength.
Technical scheme of the present invention is:
Described Continuous Flow prepares the method for type tert-butyl peroxyneo-caprate (BNP), comprises the following steps:
(1) alkaline aqueous solution is prepared for subsequent use;
(2) alkaline aqueous solution and the tertbutyl peroxide aqueous solution stably pass into 1 respectively
#react in reactor, add salt water management temperature of reaction, reactant enters 2 subsequently
#reactor;
(3) new decanoyl chloride passes into 2 solution-stabilizedly
#the product of reactor and alkaline aqueous solution and the tertbutyl peroxide aqueous solution reacts, and adds salt water management temperature of reaction;
(4) product of step (3) fully reacts further through delay lie and cools, and collects product.
Alkaline aqueous solution in described step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and alkaline aqueous solution concentration is 30-45wt%.
In described step (2), tertbutyl peroxide concentration of aqueous solution is 70-75wt%;
The flow velocity of the alkaline aqueous solution in described step (2) is 300ml/min-450ml/min, and the flow velocity of the tertbutyl peroxide aqueous solution is 60ml/min-150ml/min;
In described step (2), brine concentration is 5-10wt%, and temperature of reaction controls at 5 DEG C-15 DEG C.
In described step (3), new decanoyl chloride solution adopts purity to be the aqueous solution of 90-100wt%, preferred 98wt%;
In described step (3), the flow velocity of new decanoyl chloride solution is 100ml/min-180ml/min, and new decanoyl chloride solution adds after 30 seconds-70 seconds at alkaline aqueous solution and tertbutyl peroxide reactant aqueous solution;
In described step (3), brine concentration is 5-10wt%, and temperature of reaction controls at 15 DEG C-35 DEG C.
In described step (4), cooling temperature is 0 DEG C-10 DEG C.
Whole reaction process is 2
#in reactor, primitive reaction completes, and delay lie the raw material of a small amount of not fully reaction of effective guarantee can continue reaction; Delay lie is placed in cold water simultaneously, can cool product.
Continuous Flow of the present invention prepares the method for type tert-butyl peroxyneo-caprate (BNP), and whole process is carried out in microreactor; Particularly, realize the tertbutyl peroxide aqueous solution, basic solution and new decanoyl chloride solution Millisecond Homogeneous phase mixing in microreactor after, under the state of Continuous Flow, type tert-butyl peroxyneo-caprate (BNP) is synthesized.
Compared with prior art, its beneficial effect is in the present invention:
(1) the present invention is owing to adopting microreactor, reaction process compares traditional tank reactor, its mixing efficiency improves a lot, and due to flow speed stability, stable production process, thus constant product quality, favorable reproducibility, and waste water and discharge amount of exhaust gas significantly reduce in preparation process, labor strength is low.
(2) method preparing type tert-butyl peroxyneo-caprate (BNP) provided by the invention is carried out in microreactor, simplify technical process, overcome the complicated requirement to reactor equipment, make reaction in gentleness, safety, run continuously under the condition of environmental protection, product content and yield increase substantially, and yield can reach more than 98%.
Accompanying drawing explanation
Fig. 1 is the schema that Continuous Flow prepares the method for type tert-butyl peroxyneo-caprate (BNP).
Embodiment
Below in conjunction with drawings and Examples, the present invention is described further:
As shown in Figure 1,1
#alkaline aqueous solution in material-storage jar is through 1
#volume pump enters 1
#reactor, 2
#the tertbutyl peroxide aqueous solution in material-storage jar is through 2
#volume pump also enters 1
#reactor, enters 2 after the two hybrid reaction
#reactor; 3
#new decanoyl chloride solution in material-storage jar is through 3
#volume pump also enters 2
#reactor and the former mixture meet and react, and reacted product fully reacts further through delay lie, then enter product-collecting tank.
Embodiment 1:
(1) solid sodium hydroxide is added in deionized water, be mixed with the aqueous sodium hydroxide solution that concentration is 32%;
(2) by 1
#the flow velocity of volume pump is set to 430ml/min, and 2
#the flow velocity of volume pump is set to 120ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the tertbutyl peroxide aqueous solution of aqueous sodium hydroxide solution and 70wt% concentration enter 1 with stable flow velocity respectively
#react in reactor, the salt water management temperature of reaction simultaneously adding 5wt% concentration, at 10 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 170ml/min, 3
#volume pump is 1
#volume pump, 2
#volume pump is opened after opening 50 seconds, makes the new decanoyl chloride solution of 98wt% purity enter 2 with stable flow velocity
#the product of reactor and aqueous sodium hydroxide solution and the tertbutyl peroxide aqueous solution reacts, and adds salt water management temperature of reaction at 25 DEG C;
(4) product of step (3) continues react and be cooled to 8 DEG C through delay lie, enter product-collecting tank, static, isolate mother liquor, the crude product type tert-butyl peroxyneo-caprate (BNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type tert-butyl peroxyneo-caprate (BNP) finished product after freezing.
Embodiment 2:
(1) solid sodium hydroxide is added in deionized water, be mixed with the aqueous sodium hydroxide solution that concentration is 40%;
(2) by 1
#the flow velocity of volume pump is set to 320ml/min, and 2
#the flow velocity of volume pump is set to 80ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the tertbutyl peroxide aqueous solution of aqueous sodium hydroxide solution and 72wt% concentration enter 1 with stable flow velocity respectively
#react in reactor, the salt water management temperature of reaction simultaneously adding 7wt% concentration, at 15 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 150ml/min, 3
#volume pump is 1
#volume pump, 2
#volume pump is opened after opening 70 seconds, makes the new decanoyl chloride solution of 98wt% purity enter 2 with stable flow velocity
#the product of reactor and aqueous sodium hydroxide solution and the tertbutyl peroxide aqueous solution reacts, and adds salt water management temperature of reaction at 30 DEG C;
(4) product of step (3) fully reacts further through delay lie and is cooled to 8 DEG C, enter product-collecting tank, static, isolate mother liquor, the crude product type tert-butyl peroxyneo-caprate (BNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type tert-butyl peroxyneo-caprate (BNP) finished product after freezing.
Embodiment 3:
(1) solid potassium hydroxide is added in deionized water, be mixed with the potassium hydroxide aqueous solution that concentration is 40%;
(2) by 1
#the flow velocity of volume pump is set to 340ml/min, and 2
#the flow velocity of volume pump is set to 110ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the tertbutyl peroxide aqueous solution of potassium hydroxide aqueous solution and 75wt% concentration enter 1 with stable flow velocity respectively
#react in reactor, the salt water management temperature of reaction simultaneously adding 10wt% concentration, at 10 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 140ml/min, 3
#volume pump is 1
#volume pump, 2
#volume pump is opened after opening 40 seconds, makes the new decanoyl chloride solution of 98wt% purity enter 2 with stable flow velocity
#the product of reactor and potassium hydroxide aqueous solution and the tertbutyl peroxide aqueous solution reacts, and adds salt water management temperature of reaction at 32 DEG C;
(4) product of step (3) fully reacts further through delay lie and is cooled to 8 DEG C, enter product-collecting tank, static, isolate mother liquor, the crude product type tert-butyl peroxyneo-caprate (BNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type tert-butyl peroxyneo-caprate (BNP) finished product after freezing.
Because the technical process of above 3 embodiments all completes in microreactor, compared with traditional tank reactor, the control of microreactor is more easy to operate, charging is more accurate, therefore reacts more stable in microreactor, and then makes constant product quality, the favorable reproducibility of production.In addition, in microreactor, the contact of material is more abundant, and thus product content and yield are also high than traditional reactor.
Claims (10)
1. Continuous Flow prepares a method of type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, comprises the following steps:
(1) alkaline aqueous solution is prepared for subsequent use;
(2) alkaline aqueous solution and the tertbutyl peroxide aqueous solution stably pass into 1 respectively
#react in reactor, enter 2 subsequently
#reactor;
(3) new decanoyl chloride passes into 2 solution-stabilizedly
#the product of reactor and alkaline aqueous solution and the tertbutyl peroxide aqueous solution reacts;
(4) product of step (3) fully reacts further through delay lie and cools, and collects product.
2. Continuous Flow according to claim 1 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, alkaline aqueous solution in step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and concentration is 30-45wt%.
3. Continuous Flow according to claim 1 and 2 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, the tertbutyl peroxide concentration of aqueous solution in step (2) is 70-75wt%.
4. Continuous Flow according to claim 1 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, the flow velocity of step (2) the neutral and alkali aqueous solution is 300ml/min-450ml/min, and the flow velocity of the tertbutyl peroxide aqueous solution is 60ml/min-150ml/min.
5. the Continuous Flow according to claim 1 or 4 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, adding concentration during reaction in step (2) is that the salt water management temperature of reaction of 5-10wt% is at 5 DEG C-15 DEG C.
6. Continuous Flow according to claim 1 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, in step (3), new decanoyl chloride solution chooses the aqueous solution that purity is 90-100wt%, preferred 98wt%; Flow velocity is 100ml/min-180ml/min.
7. the Continuous Flow according to claim 1 or 6 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, in step (3), new decanoyl chloride solution adds after 30 seconds-70 seconds at alkaline aqueous solution and tertbutyl peroxide reactant aqueous solution.
8. the Continuous Flow according to claim 1 or 6 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, adding concentration during reaction in step (3) is that the salt water management temperature of reaction of 5-10wt% is at 15 DEG C-35 DEG C.
9. Continuous Flow according to claim 1 prepares the method for type tert-butyl peroxyneo-caprate (BNP), it is characterized in that, the cooling temperature in step (4) is 0 DEG C-10 DEG C.
10. prepare the method for type tert-butyl peroxyneo-caprate (BNP) according to the arbitrary described Continuous Flow of claim 1-9, it is characterized in that, whole flow process is carried out in microreactor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107698480A (en) * | 2016-08-13 | 2018-02-16 | 上海惠和化德生物科技有限公司 | A kind of continuous stream synthesis technique of the new peroxide tert-butyl caprate of no enlarge-effect |
| WO2019034006A1 (en) * | 2017-08-12 | 2019-02-21 | 上海惠和化德生物科技有限公司 | Online fully continuous flow production process for directly preparing organic peroxide from alcohol or alkane |
| CN109553560A (en) * | 2017-08-12 | 2019-04-02 | 上海惠和化德生物科技有限公司 | A kind of online Total continuity stream production technology directly preparing organic peroxide by alcohol or alkane |
| CN115385838A (en) * | 2022-07-28 | 2022-11-25 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of cumyl peroxyneodecanoate |
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| CN102442933A (en) * | 2010-10-08 | 2012-05-09 | 淄博正华助剂股份有限公司 | Preparation method of solvent type tert-butyl peroxyneo-caprate (BNP) |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107698480A (en) * | 2016-08-13 | 2018-02-16 | 上海惠和化德生物科技有限公司 | A kind of continuous stream synthesis technique of the new peroxide tert-butyl caprate of no enlarge-effect |
| WO2019034006A1 (en) * | 2017-08-12 | 2019-02-21 | 上海惠和化德生物科技有限公司 | Online fully continuous flow production process for directly preparing organic peroxide from alcohol or alkane |
| CN109553560A (en) * | 2017-08-12 | 2019-04-02 | 上海惠和化德生物科技有限公司 | A kind of online Total continuity stream production technology directly preparing organic peroxide by alcohol or alkane |
| EP3666754A4 (en) * | 2017-08-12 | 2020-08-12 | Shanghai Hybrid-Chem Technologies | Online fully continuous flow production process for directly preparing organic peroxide from alcohol or alkane |
| US10919849B2 (en) | 2017-08-12 | 2021-02-16 | Shanghai Hybrid-Chem Technologies | Online continuous flow process for the preparation of organic peroxides direct from alcohols or alkanes |
| CN115385838A (en) * | 2022-07-28 | 2022-11-25 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of cumyl peroxyneodecanoate |
| CN115385838B (en) * | 2022-07-28 | 2024-03-08 | 鄂尔多斯市瀚博科技有限公司 | Preparation method of cumyl peroxyneodecanoate |
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