CN104496874A - Method for continuous flow preparation of cumyl peroxyneodecanoate (CNP) - Google Patents
Method for continuous flow preparation of cumyl peroxyneodecanoate (CNP) Download PDFInfo
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- CN104496874A CN104496874A CN201410698419.9A CN201410698419A CN104496874A CN 104496874 A CN104496874 A CN 104496874A CN 201410698419 A CN201410698419 A CN 201410698419A CN 104496874 A CN104496874 A CN 104496874A
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- aqueous solution
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- cumyl peroxyneodecanoate
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Abstract
The invention provides a method for continuous flow preparation of cumyl peroxyneodecanoate (CNP). The method comprises the following steps that an alkaline aqueous solution is prepared, the alkaline aqueous solution and a cumyl hydroperoxide aqueous solution undergo a reaction in a reactor, a neodecanoyl chloride solution is added into the reaction product of the alkaline aqueous solution and the cumyl hydroperoxide aqueous solution, the mixture undergoes a reaction, and the reaction product further undergoes a full reaction by a delay line to produce a product, wherein the reaction processes occur in the microreactor. The solvent-type or emulsion-type cumyl peroxyneodecanoate (CNP) obtained by the method has stable product quality and good reappearance. Through use of the microreactor, technical processes are simplified, the reactions continue under the mild, safe and eco-friendly conditions, product content and a product yield are greatly improved and the yield is more than 97.5%.
Description
Technical field
The present invention relates to the preparation method of the initiator cumyl peroxyneodecanoate (CNP) of a kind of superpolymer synthesis, particularly a kind of Continuous Flow prepares the method for cumyl peroxyneodecanoate (CNP), 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.Cumyl peroxyneodecanoate (CNP) as a kind of Macroscopic single crystal higher effective initiator, compared with common azo-initiator, in superpolymer polymerization process, consumption is few, and efficiency of initiation is high, and polyreaction heat release is even, product performance are excellent, the huge market demand.
Industrialization cumyl peroxyneodecanoate (CNP) 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 cumyl peroxyneodecanoate (CNP) 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 cumyl peroxyneodecanoate (CNP), 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 cumyl peroxyneodecanoate (CNP), comprises the following steps:
(1) alkaline aqueous solution is prepared for subsequent use;
(2) alkaline aqueous solution and the hydrogen phosphide cumene 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 hydrogen phosphide cumene 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 35-55wt%.
In described step (2), hydrogen phosphide cumene concentration of aqueous solution is 70-75wt%;
The flow velocity of the alkaline aqueous solution in described step (2) is 250ml/min-400ml/min, and the flow velocity of the hydrogen phosphide cumene aqueous solution is 80ml/min-170ml/min;
In described step (2), brine concentration is 5-10wt%, and temperature of reaction controls at 10 DEG C-35 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-210ml/min, and new decanoyl chloride solution adds after 20 seconds-60 seconds at alkaline aqueous solution and hydrogen phosphide cumene reactant aqueous solution;
In described step (3), brine concentration is 5-10wt%, and temperature of reaction controls at 20 DEG C-40 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 cumyl peroxyneodecanoate (CNP), and whole process is carried out in microreactor; Particularly, realize the hydrogen phosphide cumene aqueous solution, basic solution and new decanoyl chloride solution Millisecond Homogeneous phase mixing in microreactor after, under the state of Continuous Flow, cumyl peroxyneodecanoate (CNP) 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 cumyl peroxyneodecanoate (CNP) 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 97.5%.
Accompanying drawing explanation
Fig. 1 is the schema that Continuous Flow prepares the method for cumyl peroxyneodecanoate (CNP).
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 hydrogen phosphide cumene 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 35%;
(2) by 1
#the flow velocity of volume pump is set to 350ml/min, and 2
#the flow velocity of volume pump is set to 90ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the hydrogen phosphide cumene 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 15 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 190ml/min, 3
#volume pump is 1
#volume pump, 2
#volume pump is opened after opening 30 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 hydrogen phosphide cumene 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 5 DEG C, enter product-collecting tank, static, isolate mother liquor, the crude product cumyl peroxyneodecanoate (CNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type cumyl peroxyneodecanoate (CNP) 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 300ml/min, and 2
#the flow velocity of volume pump is set to 110ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the hydrogen phosphide cumene 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 20 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 200ml/min, 3
#volume pump is 1
#volume pump, 2
#volume pump is opened after opening 20 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 hydrogen phosphide cumene aqueous solution reacts, and adds salt water management temperature of reaction at 35 DEG C;
(4) product of step (3) fully reacts further through delay lie and is cooled to 3 DEG C, enter product-collecting tank, static, isolate mother liquor, the crude product cumyl peroxyneodecanoate (CNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type cumyl peroxyneodecanoate (CNP) 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 330ml/min, and 2
#the flow velocity of volume pump is set to 100ml/min, opens 1 simultaneously
#volume pump, 2
#volume pump, makes the hydrogen phosphide cumene 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 18 DEG C, enters 2 subsequently
#reactor;
(3) 3 are set
#the flow velocity of volume pump is 160ml/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 potassium hydroxide aqueous solution and the hydrogen phosphide cumene aqueous solution reacts, and adds salt water management temperature of reaction at 35 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 cumyl peroxyneodecanoate (CNP) obtained, through salt water washing, is mixed with certain density solvent-borne type or emulsion type cumyl peroxyneodecanoate (CNP) 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 cumyl peroxyneodecanoate (CNP), it is characterized in that, comprises the following steps:
(1) alkaline aqueous solution is prepared for subsequent use;
(2) alkaline aqueous solution and the hydrogen phosphide cumene 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 hydrogen phosphide cumene 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 cumyl peroxyneodecanoate (CNP), it is characterized in that, alkaline aqueous solution in step (1) is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and concentration is 35-55wt%.
3. Continuous Flow according to claim 1 and 2 prepares the method for cumyl peroxyneodecanoate (CNP), it is characterized in that, the hydrogen phosphide cumene concentration of aqueous solution in step (2) is 70-75wt%.
4. Continuous Flow according to claim 1 prepares the method for cumyl peroxyneodecanoate (CNP), it is characterized in that, the flow velocity of step (2) the neutral and alkali aqueous solution is 250ml/min-400ml/min, and the flow velocity of the hydrogen phosphide cumene aqueous solution is 80ml/min-170ml/min.
5. the Continuous Flow according to claim 1 or 4 prepares the method for cumyl peroxyneodecanoate (CNP), 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 10 DEG C-35 DEG C.
6. Continuous Flow according to claim 1 prepares the method for cumyl peroxyneodecanoate (CNP), 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-210ml/min.
7. the Continuous Flow according to claim 1 or 6 prepares the method for cumyl peroxyneodecanoate (CNP), it is characterized in that, in step (3), new decanoyl chloride solution adds after 20 seconds-60 seconds at alkaline aqueous solution and hydrogen phosphide cumene reactant aqueous solution.
8. the Continuous Flow according to claim 1 or 6 prepares the method for cumyl peroxyneodecanoate (CNP), 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 20 DEG C-40 DEG C.
9. Continuous Flow according to claim 1 prepares the method for cumyl peroxyneodecanoate (CNP), it is characterized in that, the cooling temperature in step (4) is 0 DEG C-10 DEG C.
10. Continuous Flow according to claim 1 prepares the method for cumyl peroxyneodecanoate (CNP), it is characterized in that, whole flow process is carried out in microreactor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693584A (en) * | 2016-03-17 | 2016-06-22 | 乌鲁木齐市华泰隆化学助剂有限公司 | Peroxided neodecanoic acid isopropyl phenyl ester and method for preparing peroxided neodecanoic acid isopropyl phenyl ester through phase transfer catalyst |
| CN112608265A (en) * | 2020-12-03 | 2021-04-06 | 宁夏顺邦达新材料有限公司 | Production process of cumyl peroxyneodecanoate |
| 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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| JP2006089472A (en) * | 2004-08-27 | 2006-04-06 | Asahi Glass Co Ltd | Method for producing organic peroxide |
| CN101287704A (en) * | 2005-10-14 | 2008-10-15 | 埃尔费尔德微技术Bts有限责任公司 | Method for the production of organic peroxides by means of a microreaction technique |
| CN101641326A (en) * | 2006-07-12 | 2010-02-03 | 联合引发剂有限责任两合公司 | Continuous method for producing acyl peroxides |
| CN102443079A (en) * | 2010-10-08 | 2012-05-09 | 淄博正华助剂股份有限公司 | Preparation method of solvent type cumyl peroxyneodecanoate (CNP) |
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- 2014-11-26 CN CN201410698419.9A patent/CN104496874A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006089472A (en) * | 2004-08-27 | 2006-04-06 | Asahi Glass Co Ltd | Method for producing organic peroxide |
| CN101287704A (en) * | 2005-10-14 | 2008-10-15 | 埃尔费尔德微技术Bts有限责任公司 | Method for the production of organic peroxides by means of a microreaction technique |
| CN101641326A (en) * | 2006-07-12 | 2010-02-03 | 联合引发剂有限责任两合公司 | Continuous method for producing acyl peroxides |
| CN102443079A (en) * | 2010-10-08 | 2012-05-09 | 淄博正华助剂股份有限公司 | Preparation method of solvent type cumyl peroxyneodecanoate (CNP) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693584A (en) * | 2016-03-17 | 2016-06-22 | 乌鲁木齐市华泰隆化学助剂有限公司 | Peroxided neodecanoic acid isopropyl phenyl ester and method for preparing peroxided neodecanoic acid isopropyl phenyl ester through phase transfer catalyst |
| CN112608265A (en) * | 2020-12-03 | 2021-04-06 | 宁夏顺邦达新材料有限公司 | Production process of cumyl peroxyneodecanoate |
| 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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Application publication date: 20150408 |