CN105541689B - A kind of 2,5 dimethyl 2,5 pairs（Tert-butyl peroxide）The purification system and technique of hexane - Google Patents
A kind of 2,5 dimethyl 2,5 pairs（Tert-butyl peroxide）The purification system and technique of hexane Download PDFInfo
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- CN105541689B CN105541689B CN201610039588.0A CN201610039588A CN105541689B CN 105541689 B CN105541689 B CN 105541689B CN 201610039588 A CN201610039588 A CN 201610039588A CN 105541689 B CN105541689 B CN 105541689B
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- C07C407/00—Preparation of peroxy compounds
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Abstract
The invention discloses a kind of 2,5 dimethyl 2,5 pairs（Tert-butyl peroxide）The purification system of hexane, including distillation still, decolouring kettle；Distillation still is connected by feeding pipe with decolouring kettle；Distillation still includes housing, is provided with housing into blank pipe, and it is 10~200mm to enter one end of blank pipe and the distance from bottom of housing, and the roof of the other end and housing that enter blank pipe connects, and the setting for entering blank pipe is beneficial to be passed through air into liquid, aids in fast liquid boiling；Decolouring kettle is set, improves product quality；The present invention also provides a kind of 2,5 dimethyl 2,5 pairs（Tert-butyl peroxide）The purifying technique of hexane, is distilled under the conditions of 61~68 DEG C, 0.093~0.098MPa, and air is passed through into liquid and is distilled, and distillation is decolourized after terminating to product, shortens distillation time, improves the purity and colourity of target product, reduces purification energy consumption, material consumption.
Description
Technical field
The present invention relates to chemicals technical field, and in particular to 2,5- of one kind dimethyl -2,5- is double（The tertiary fourth of peroxidating
Base）The purification system and technique of hexane.
Background technology
2,5- dimethyl -2,5 pair（Tert-butyl peroxide）Hexane, also known as 2,5- dimethyl -2,5 pair（T-butylperoxy）
Hexane, it " 2,5 " vulcanizing agents, is industrial important peroxide to be commonly called as double.Its molecular formula is C16H34O4, molecular weight is
290.44 density 0.847g/cm3, proportion D（20℃）0.865, index of refraction 1.4185, flash-point is：Remain silent 36 DEG C, be open
58℃；Alarm temperature is 75 DEG C, and SADT is 80 DEG C, theoretical active oxygen content 11.02%, is a kind of inflammable, easy
Quick-fried, odorless, pale yellow transparent oily liquids.2,5- dimethyl -2,5- are double（Tert-butyl peroxide）Hexane is usually used in polymerizeing
The free-radical initiator of journey and the viscosity for improving polyolefin；Silicon rubber vulcanization product is also used for, because tensile strength and hardness are equal
Height, extends and compression is relatively low, can be used for effective high temperature vulcanized dose of vinyl rubber, unsaturated polyester (UP) curing agent and
Vulcanizing agent of fluorubber, polyurethane rubber and the glue of second third etc..
2,5- dimethyl -2,5- are double（T-butylperoxy）The synthesis of hexane is anti-using peroxidization and tert-butylation
Should.Peroxidization under the catalysis of the concentrated sulfuric acid, is first synthesized for raw material with 2,5- dimethyl -2,5- hexylene glycol and hydrogen peroxide
The peroxidase 12 of 2,5- dimethyl -2,5- hexylene glycols, 5- dimethyl -2,5- butylperoxyhexanes, peroxide are complete with the tert-butyl alcohol again
Into tertiary butyl reaction, it is double to produce 2,5- dimethyl -2,5-（T-butylperoxy）Hexane crude product.
It is existing double to 2,5- dimethyl -2,5-（Tert-butyl peroxide）The method that hexane is purified mainly has：At 40 DEG C
~60 DEG C, under the conditions of -0.09MPa~-0.1MPa, it is double to 2,5- dimethyl -2,5-（Tert-butyl peroxide）Lead in hexane crude product
Enter nitrogen to be evaporated under reduced pressure, it is double to obtain 2,5- dimethyl -2,5-（Tert-butyl peroxide）Hexane, and obtained after being evaporated under reduced pressure
Product is not decolourized using activated carbon.It is double to 2,5- dimethyl -2,5- using the technical scheme（Tert-butyl peroxide）Oneself
During alkane is purified, the equipment that is passed through nitrogen, it can continue to continue to use the distillation still structure in existing equipment for purifying, but purify
Distillation time is relative to be extended, and influences target product purity；Decolouring kettle is not used in existing equipment for purifying to 2,5- dimethyl -2,5-
It is double（Tert-butyl peroxide）Hexane is decolourized, and causes final finished colour difference, and contains more impurity in product, is unable to reach
The quality requirements of product；Nitrogen is passed through in distillation still in existing purifying technique, makes 2,5- dimethyl -2,5- double（Peroxidating uncle
Butyl）Hexane semi-finished product seethe with excitement, but nitrogen needs to purify before being passed through, and increase cost for purification；And the condition of purifying technique is 40
~60 DEG C, -0.09MPa~-0.1MPa, wherein temperature setting are only capable of meeting the requirement to heating distillation, can not be to 2,5- bis-
Methyl -2,5- is double（Tert-butyl peroxide）The boiling of hexane plays a driving role, and some compositions can not distill in liquid, target
Product purity is low；Distilled simultaneously under -0.1MPa pressure, be difficult to reality in vacuum distillation to those skilled in the art
It is existing.
Existing 2,5- dimethyl -2,5- is double based on more than（Tert-butyl peroxide）Hexane purifying plant, it is technologic lack
Fall into, it is double that research and development devise 2,5- of one kind dimethyl -2,5-（Tert-butyl peroxide）The purification system and technique of hexane.
The content of the invention
The technical problems to be solved by the invention are：The distillation still used in purifier apparatus, it is passed through the structure of nitrogen and led
Cause cost for purification increase；The device not decolourized to the product after distillation, causes final product colour difference, and quality is low；
Purpose is：It is double to provide 2,5- of one kind dimethyl -2,5-（Tert-butyl peroxide）The purification system of hexane, it is provided with using interior into sky
The distillation still structure of pipe, it is double to solve 2,5- of purification dimethyl -2,5-（Tert-butyl peroxide）Used in hexane device and be passed through nitrogen
The problem of infrastructure cost is high；Set decolouring kettle structure to decolourize the product after distillation, solve the defects of product colour difference.
Another technical problem to be solved by this invention is：Existing purifying technique is used at 40~60 DEG C, -0.09MPa
It is evaporated under reduced pressure under the conditions of~-0.1MPa, can not be realized wherein -0.1MPa is operated for those skilled in the art；Using logical
Enter the method for nitrogen distillation, nitrogen needs to purify before being passed through, and increases cost of material；At 40~60 DEG C, in liquid some impurity into
Dividing sufficiently to be distilled, and make final products purity low；Another object of the present invention is to：One kind 2,5- diformazans are provided
Base -2,5- is double（Tert-butyl peroxide）The purifying technique of hexane, using in 61~68 DEG C, -0.093MPa~-0.098MPa conditions
It is lower double to 2,5- dimethyl -2,5-（Tert-butyl peroxide）Air is passed through in hexane semi-finished product to be distilled, and solves existing process
In be passed through nitrogen cost height, distillation time length, the problems such as target product purity is low.
The present invention's is achieved through the following technical solutions：
2,5- of one kind dimethyl -2,5- is double（Tert-butyl peroxide）The purification system of hexane, including distillation still, decolouring kettle；
Distillation still is connected by feeding pipe with decolouring kettle；Distillation still includes housing, is provided with housing into blank pipe, enter one end of blank pipe with
The distance from bottom of housing is 10~200mm, and the roof of the other end and housing that enter blank pipe connects.
Distillation still is connected by feeding pipe with decolouring kettle, i.e., the discharging mouth of pipe is provided with the bottom of distillation still, and discharge the mouth of pipe
It is connected by feeding pipe with the import of decolouring kettle.The effect of decolouring kettle is that product is decolourized, and improves product colourity.Decolourize
Kettle also known as decoloring reaction kettle, it is the common equipment of chemical field, the decolouring as the rich sharpening work Machinery Co., Ltd. in Weihai produces is anti-
Answer kettle.
Set in distillation still into blank pipe, it is stainless steel tube to enter blank pipe, and the main function for entering blank pipe is as to 2,5- bis-
Methyl -2,5- is double（Tert-butyl peroxide）The pipeline of air is passed through in hexane liquid, under air effect power, 2,5- dimethyl-
2,5- is double（Tert-butyl peroxide）Hexane seethes with excitement, and starts to distill, air is not required to purify before being passed through, wide material sources.
It is 10~200mm to enter one end of blank pipe and the distance from bottom of housing, enters insertion position and liquid level or the housing of blank pipe
Distance from bottom relatively closely can influence liquid boiling degree.That enters blank pipe insertion liquid is closely located to liquid surface, and air is to insertion
The active force of site fluid is strong around position, and water vapour, the impurity liquid energy being dissolved in this partially liq are rapid evaporated,
The impurity liquid boiling degree of the latter half is low, needs the long period evaporated from distillation still；Similarly, when insertion position connects
During nearly housing bottom, air effect power is largely acted on housing, is delivered to the active force of liquid top half and is reduced, liquid
Boiling degree reduces, and distillation time extends.The above analysis, enter one end that blank pipe is located in distillation still raw material liquid level and housing
Distance from bottom is 10~200mm, is that technical staff considers distillation still specification, inventory and enters blank pipe insertion raw material liquid level
The factors such as influence of the interior length to liquid boiling degree and many experiments draw, it is normal not to be that those skilled in the art are readily apparent that
Advise number range or replacement.The distance from bottom for entering blank pipe and housing is not defined in the prior art, also not to this
The relation of distance and distillation time length, target product purity makees deep experimental study.Therefore, research is drawn：Blank pipe will be entered
10~200mm is arranged to the distance from bottom of housing, the boiling degree of liquid can be strengthened, shortens the distillation that liquid reaches predetermined concentration
Time, the purity of target product is improved, reduce the material loss in still-process.
Further, in order to preferably realize the present invention, the top of the decolouring kettle is provided with activated carbon charging device.Activity
Storage device of the charcoal charging device as activated carbon, when needing to decolourize to product, the roof import directly from decolouring kettle
Into stirring is decolourized.
Further, in order to preferably realize the present invention, it is provided with what is connected with enclosure interior on the roof of the housing
Gas-adding pipe.Gas-adding pipe effect is after distillation terminates, and the compressed air outside housing is delivered in housing, in the work of compressed air
Product is pressed into decolouring kettle under firmly.
Further, in order to preferably realize the present invention, it is described enter blank pipe other end end be provided with needle valve.Needle valve
Enter the switching device of blank pipe for control air.With needle-like valve action identical technical equivalents in the technical program, such as
Control valve, within the scope of the present invention.
Further, in order to preferably realize the present invention, it is described enter blank pipe number be 2~4, and to steam in housing
The central shaft for evaporating kettle is uniformly and symmetrically distributed for axle.The number for entering blank pipe is 1~4,1 when entering blank pipe, as long as meeting into blank pipe
One end insertion housing raw material liquid level in, enter blank pipe the other end and housing roof connect.It is preferred that enter blank pipe for 2~4
Root, when entering blank pipe number 2,2 lower end lines for entering blank pipe are parallel as axle and right with upper end line using the central shaft of distillation still
Claim；When entering blank pipe number 3, the equilateral triangle of 3 equilateral triangles for entering blank pipe lower end composition and upper end composition is with distillation still
Central shaft is axle parallel and symmetrical；When entering blank pipe number 4,4 lower ends entered in blank pipe in liquid levels to be purified connect
The square that the square connect is formed by connecting with upper end is using the central shaft of distillation still as axle parallel and symmetrical.It is right above
Enter the setting of blank pipe number, main function is to increase the air capacity being passed through in liquid to be purified, journey of being seethed with excitement in liquid to be purified
Degree is strengthened and boiling degree is uniform, the evaporation of accelerating impurity liquid and moisture.
Further, in order to preferably realize the present invention, the outlet at bottom of the decolouring kettle passes through feeding pipe and suction filtration
Device connects.The effect of Suction filtration device is that 2,5- dimethyl -2,5- that decolouring kettle decolourizes out is double（Tert-butyl peroxide）Oneself
The mixture of alkane and activated carbon filters separation, and it is double to produce 2,5- dimethyl -2,5- after purification（Tert-butyl peroxide）Hexane.
It is double that the present invention still further provides 2,5- of one kind dimethyl -2,5-（Tert-butyl peroxide）The purifying technique of hexane,
It is achieved through the following technical solutions：
2,5- dimethyl -2,5- is double（Tert-butyl peroxide）In hexane semi-finished product suction distillation still, heating distillation still is extremely
Constant temperature after 61 DEG C~68 DEG C of temperature in the kettle；
In heating process, it is in negative pressure to make in distillation still, opens needle valve, is passed through air, and 2,5- dimethyl -2,5- are double（Cross
Aoxidize the tert-butyl group）Hexane is in fluidized state under air effect power, starts to distill, qualified to sampling analysis product design, is stopped
Distillation；
Product in distillation still is pressed into decolouring kettle, adds decolorising agent, stirring, to sampling analysis product 2,5- dimethyl -2,
5- is double（Tert-butyl peroxide）Hexane colourity is qualified, produces.
Wherein, make to vacuumize realization by vavuum pump in negative pressure in distillation still, specific vavuum pump can be Roots vacuum
Pump.
For the ease of 2,5- dimethyl -2,5- in distillation still is double（Tert-butyl peroxide）The press-in of hexane product is decolourized
Kettle, can be passed through compressed air into distillation still by gas-adding pipe, product is rapidly entered distillation still by inner air and outer air pressure.To
The decolorising agent added in decolouring kettle can be activated carbon, and activated carbon is storable in activated carbon charging device.Wherein, activated carbon is thrown
Expect the position of device, can be set as needed, such as may be provided at the roof of decolouring kettle, roof is provided with can be by activated carbon
Charging device, the switching device of decolouring kettle connection or import.
It is first that 2,5- dimethyl -2,5- in distillation still is double in the purifying technique（Tert-butyl peroxide）Hexane liquid adds
For heat to 61~68 DEG C, and in heating process, it is in negative pressure to make in distillation still.The wherein selection of heating-up temperature, and in the prior art
40~60 DEG C are compared, beneficial to boiling point under atmospheric pressure is evaporated for 61~68 DEG C of impurity liquid.2,5- dimethyl -2,5-
It is double（Tert-butyl peroxide）The alarm temperature of hexane is 75 DEG C, and SADT is 80 DEG C, and 40~60 DEG C of temperature ranges
Setting only meet processing safety, and 61~68 DEG C of selection on the premise of safe operation is met, can prevent raw material
Decompose, and can be effectively evaporated for 61~68 DEG C and 68~74 DEG C of impurity liquid by atmospheric pressure boiling point.Under negative pressure, from
For the impurity component angle being evaporated, liquid is heated to 61~68 DEG C of ratios and is heated to 40~60 DEG C of impurity being evaporated
Component amount is big, species is more；Consider from liquid boiling degree, liquid is heated to 61~68 DEG C of ratios and is heated to 40~60 DEG C of boiling degree more
Greatly, and each several part boiling degree it is uniform, therefore 61~68 DEG C to be more conducive to 2,5- dimethyl -2,5- double（Tert-butyl peroxide）Oneself
Alkane purifies, and shortens the distillation time for reaching predetermined concentration, and the product purity finally purified is higher.
Do not account in the prior art double to the product 2 after distillation, 5- dimethyl -2,5- by decolouring kettle（Peroxidating uncle
Butyl）Hexane is decolourized, therefore final products surface is often stained with impurity or coloring matter, or color and luster muddiness, lightness
Low, poor quality, aesthetic property is strong.
And by the mode decolourized can be by a variety of in product press-in decolouring kettle in distillation still in the technical program, can be with
Using the pressure difference inside and outside distillation still, that is, breather pipe is opened, compressed air is passed through by breather pipe.
As long as the decolorising agent added in the technical program meets that the impurity thing on product can be adsorbed, the color of product is improved
Pool.
Further, in order to preferably realize the present invention, in the heating process, in distillation still vacuum for-
0.093MPa~-0.098MPa；The distillation time is 7.5~8.5 hours.
Negative pressure is carried out preferably herein, vacuum is -0.093MPa~-0.098MPa in distillation still, and in the prior art
Only with the vacuum ranges of a routine, such as -0.09MPa~-0.1MPa, it is only capable of meeting to be evaporated under reduced pressure, being easy to will be extraneous empty
Gas is passed through in liquid level.And herein to the preferred of vacuum ranges, meet to be evaporated under reduced pressure same, beneficial to being passed through outside air, also
Distillation time, target product purity directly with distillation still is relevant.Wherein, the change of vacuum and heating process are same in distillation still
Shi Jinhang, with the change of vacuum, the boiling point of liquid also changes therewith, and the impurity component, moisture in liquid evaporate therewith,
During this, distillation time shortens, the purity increase of target product；With the increase of temperature, the boiling degree of liquid is strengthened,
Distillation still is under the negative pressure constantly reduced, and the boiling point of various composition gradually reduces in liquid, more conducively impurities in liquid composition
Evaporation, the concentration increase of liquid to be purified, the time for reaching predetermined concentration shorten, and the purity of final products is higher.
It is double from 2,5- dimethyl -2,5-（Tert-butyl peroxide）When hexane is in fluidized state, start to distill, distillation 7.5-
It can reach predetermined product design within 8.5 hours.Further preferred 8 hours of distillation time, selects the distillation time, product purity
98% is can reach, product material loss can be reduced to 0.8%.
Further, in order to preferably realize the present invention, the mixing time is 20~40 minutes, in decolorization,
It is double to be sufficiently stirred 2,5- dimethyl -2,5-（Tert-butyl peroxide）The mixture of hexane and activated carbon, charcoal absorption product institute
Colored substance of carrying etc., obtained product color is bright, penetrating, meets needs and the product standard requirement of client.
Further, it is described to suck 2,5- dimethyl -2,5- pair in distillation still in order to preferably realize the present invention（Peroxide
Change the tert-butyl group）The amount of hexane is the 50~65% of distillation still volume.
2,5- dimethyl -2,5- are double（Tert-butyl peroxide）Hexane, which enters distillation still, to be realized by Roots vaccum pump.2,
5- dimethyl -2,5- is double（Tert-butyl peroxide）The raw material volume that hexane enters in distillation still, it is relevant with the specification of distillation still.Its
Middle distillation still is common equipment in industry, and specification determines.Raw material volume is arranged on the 50~65% of distillation still volume, meet into
One end of blank pipe is located in liquid level, and meets simultaneously into the distance of blank pipe and housing in the range of 10~200mm, is boiled beneficial to liquid
Rise, shorten distillation time, reduce the content of impurities in liquid composition.
The present invention compared with prior art, has the following advantages and advantages：
（1）The present invention 2,5- of purification dimethyl -2,5- is double（Tert-butyl peroxide）In the system of hexane, set in distillation still
Put into blank pipe, as the passage that air is passed through into distillation kettle liquid body, it is double to play 2,5- of auxiliary dimethyl -2,5-（The tertiary fourth of peroxidating
Base）The effect of hexane boiling, shortens distillation time.
（2）Decolouring kettle is used in purification system of the present invention, 2,5- dimethyl -2,5- after handling distillation is double（Peroxidating
The tert-butyl group）Hexane decolourizes, and improves the bright of its colourity, permeability.
（3）Purification system of the present invention is easy to operation, can effectively improve the qualities such as purity, the colourity of target product.
（4）2,5- of present invention dimethyl -2,5- is double（Tert-butyl peroxide）Used in the purifying technique of hexane and be passed through air,
Air can be passed directly into compared with nitrogen, wide material sources, be not required to purify.
（5）2,5- of present invention dimethyl -2,5- is double（Tert-butyl peroxide）Activated carbon pair is used in the purifying technique of hexane
Product is stirred decolouring, improves the color of product, quality.
（6）2,5- of present invention dimethyl -2,5- is double（Tert-butyl peroxide）The purifying technique of hexane be 61~68 DEG C ,-
Distilled under the conditions of 0.093MPa~-0.098MPa, evaporated beneficial to product boiling and impurity liquid, do not cause target product point
Solution, it is easy to operate, it is easy to implement.
（7）Purifying technique of the present invention, distilation can be accelerated, shorten distillation time, improve target product
Purity, reduce material loss caused by purification.
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding the embodiment of the present invention, forms one of the application
Point, do not form the restriction to the embodiment of the present invention.In the accompanying drawings：
Fig. 1 is schematic structural view of the invention；
Fig. 2 is the structural representation of distillation still in the present invention；
Fig. 3 is the structural representation of the embodiment of the present invention 4；
Mark and corresponding parts title in accompanying drawing：
The 1- charging mouths of pipe, the 2- discharging mouths of pipe, 3- chuck water inlet pipes, 4- chuck outlet pipes, 5- chuck heating rods, 6- enter sky
Pipe, 7- needle valves, 8- pressure vacuum gauges, 9- temperature in the kettle meter probe, 10- gas-adding pipes, 11- jacket temperatures meter probe, 12- distillations
Kettle chuck, 13- housings, 21- distillation stills, 22- decolouring kettles, 23- destilling towers, 24- condensers, 25- collecting tanks, 26- Suction filtration devices,
27- air compressor machines, 28- vavuum pumps, 29- Roots vaccum pumps, 30- high position measuring tanks, the measuring tanks of 31- second, the filtering dresses of 32- second
Put, 33- finished product storage devices, the filters of 34- first, the measuring tanks of 35- first.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment and accompanying drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make
For limitation of the invention.
Embodiment 1：
As shown in Figure 1 and Figure 2,2,5- of one kind dimethyl -2,5- is double（Tert-butyl peroxide）The purification system of hexane, including
Distillation still 21, decolouring kettle 22；Distillation still 21 is connected by feeding pipe with decolouring kettle 22；Distillation still 21 includes housing 13, housing
It is provided with that into blank pipe 6, to enter one end of blank pipe 6 and the distance from bottom of housing 13 be 10mm in 13, enters the other end and housing 13 of blank pipe 6
Roof connection.
The top of decolouring kettle 22 is provided with activated carbon charging device.
The gas-adding pipe 10 connected with the inside of housing 13 is installed on the roof of housing 13.
The other end end for entering blank pipe 6 is provided with needle valve 7.
Enter 6 numbers of blank pipe for 2, and be uniformly and symmetrically distributed in housing 13 using the central shaft of distillation still 21 as axle.
The outlet at bottom of the decolouring kettle 22 is connected by feeding pipe with Suction filtration device 26.
Purification system also includes destilling tower 23, condenser 24, collecting tank 25, and the roof of distillation still 21 is provided with steam (vapor) outlet,
Steam (vapor) outlet is connected by conveyance conduit with the bottom inlet of destilling tower 23, and the top exit of destilling tower 23 passes through air shooter
Road is connected with condenser 24, and condenser 24 is connected with collecting tank 25, and the collection of collecting tank 25 condenses impurity and moisture mixing is useless
Liquid.
Destilling tower 23 is that moisture and other impurity liquids to being come out from the evaporated on top of distillation still 21 etc. carry out second distillation,
The waste heat brought out from distillation still 21 is made full use of during second distillation.
Condenser 24 cools down the water vapour distilled from destilling tower 23 and other foreign gases, and enters in collecting tank 25
Storage.
Wherein condenser 24, collecting tank 25 are connected with Roots vaccum pump 29, are evaporated under reduced pressure due to being used in the present embodiment,
Pressure subatmospheric in condenser 24, incoagulable gas in system is extracted out by the effect of Roots vaccum pump 29, maintain one
The condensed environment of individual negative relative.Collecting tank 25 is to reduce the internal pressure of collecting tank 25 with the main function that Roots vaccum pump 29 is connected
Power, it is easy to collect the liquid condensed in condenser 24 into collecting tank 25.The choosing of Roots vaccum pump 29 in the present embodiment
Select only preferably, the other structures equivalent with Roots vaccum pump 29 can also be used, as long as meeting to liquid waste after purification
Processing.
Purification system also includes the first measuring tank 35, the material outlet of decolouring kettle 22 with successively with Suction filtration device 26, first
Measuring tank 35 connects.
Filtered product can be stored directly after the metering of the first measuring tank 35.
Purification system also includes high-order measuring tank 30, the first filter 34, the second measuring tank 31, the second filter
32nd, finished product storage device 33, the top entry of high-order measuring tank 30 are connected with the outlet at bottom of the first measuring tank 35, high position metering
Tank 30 is connected with the first filter 34, the second measuring tank 31, the second filter 32, finished product storage device 33 successively.
First measuring tank 35 is connected to air compressor machine 27 and vavuum pump 28.
In large-scale production, the amount of storage of each measuring tank is limited, and, it is necessary to count when measuring tank storage time is longer
Transferred product is carried out between measuring tank.The product in first measuring tank 35 is pressed into height in the presence of air compressor machine 27, vavuum pump 28
Impurity substances in product are filtered, improve the purity of product, reduction is deposited by position measuring tank 30 through the first filter 34
Caused impurity in storage, transfer, metering process.
Enter the second measuring tank 31, the effect of the second measuring tank 31 and the first metering after the processing of the first filter 34
The effect of tank 35 is identical, is primarily to facilitate product and is shifted, stored between measuring tank.
As needed, the first measuring tank 35 can also connect the second filter 32, the second filter 32 and the first mistake
It is identical to filter the effect of device 34, is ultimately stored in finished product storage device 33.
The outer wall of the housing 13 is provided with the pressure vacuum gauge 8 for being used for monitoring and show pressure change in housing 13, shell
The latter half of body 13 is coated with distillation still chuck 12, and chuck water inlet pipe 3, chuck outlet pipe are respectively equipped with distillation still chuck 12
4；It is provided with chuck heating rod 5 in distillation still chuck 12, number at least six of chuck heating rod 5, is provided with distillation still chuck 12
Jacket temperature meter probe 11, the bottom of housing 13 are provided with the charging mouth of pipe 1, temperature in the kettle meter probe 9 are provided with housing 13.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 97.5%, steam
It is 8 hours to evaporate the time, supplies consumption 1.4%.
Embodiment 2：
The one end for entering blank pipe 6 and the distance from bottom of housing 13 are arranged to by the present embodiment on the basis of embodiment 1
100mm, enter 6 numbers of blank pipe for 3, other technical characteristics are identical with the architectural feature in embodiment 1, repeat no more.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 98.1%, steam
The time is evaporated for 8 hours, and supplies consumption is 0.9 %.
Embodiment 3：
The one end for entering blank pipe 6 and the distance from bottom of housing 13 are arranged to by the present embodiment on the basis of embodiment 1
200mm, enter 6 numbers of blank pipe for 4, other technical characteristics are identical with the architectural feature in embodiment 1, repeat no more.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 98%, distillation
Time is 7.5 hours, supplies consumption 1.0%.
Embodiment 4：
The present embodiment on the basis of above-described embodiment, as shown in figure 3, air compressor machine 27 also respectively with distillation still 21, second
Measuring tank 31 connects, and air compressor machine 27 is the pressure generator of compressed air, is known to the skilled person device.In this reality
Applying the main function of air compressor machine 27 in example is：1）By 2,5- dimethyl -2,5- pair that distillation is completed in distillation still 21（Peroxidating
The tert-butyl group）In hexane press-in decolouring kettle 22；2）For 2,5- dimethyl -2,5- in the second measuring tank 31 is double（The tertiary fourth of peroxidating
Base）Hexane is transferred to finished product storage device 33 and provides power.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 98.5%, steam
It is 7.8 hours to evaporate the time, supplies consumption 1.1%.
Embodiment 5：
2,5- of one kind dimethyl -2,5- is double（Tert-butyl peroxide）The purifying technique of hexane, concrete operation step are：
2,5- dimethyl -2,5- is double（Tert-butyl peroxide）In hexane semi-finished product suction distillation still 21, the amount of suction is
The 50% of distillation still volume, constant temperature after heating distillation still 21 to 61 DEG C of temperature in the kettle；
In heating, it is -0.093MPa to make vacuum in distillation still 21, opens needle valve 7, is passed through into distillation kettle liquid body
Air, 2,5- dimethyl -2,5- are double（Tert-butyl peroxide）Hexane is in fluidized state under air effect power, starts to distill, and is steamed
Evaporate 7.5 hours, sampling analysis product design is qualified, stops distillation；
Gas-adding pipe 10 is opened, compressed air is passed through and product in distillation still 21 is pressed into decolouring kettle 22, activated carbon feeds intake dress
Put and activated carbon is added into decolouring kettle 22, stir 20min, sampling analysis product 2,5- dimethyl -2,5- pair（The tertiary fourth of peroxidating
Base）Hexane colourity is qualified, produces.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 97.6%, steam
It is 7.5 hours to evaporate the time, supplies consumption 0.9%.
Embodiment 6：
It is on the basis of embodiment 5,2,5- dimethyl -2,5- is double（Tert-butyl peroxide）On the basis of hexane purifying technique
It is preferred that：The semi-finished product amount of suction is the 60% of distillation still volume, and vacuum be -0.098MPa in kettle, and temperature is 68 DEG C, during distillation
Between be 8 hours, in decolouring kettle stir bleaching time be 30min, other techniques are in the same manner as in Example 4, repeat no more.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 97.8%, steam
It is 7.6 hours to evaporate the time, supplies consumption 1.1%.
Embodiment 7：
It is on the basis of embodiment 5,2,5- dimethyl -2,5- is double（Tert-butyl peroxide）On the basis of hexane purifying technique
It is preferred that：65% that semi-finished product amount is distillation still volume is sucked, vacuum is -0.095MPa in kettle, and temperature is 65 DEG C, distillation time
For 8.5 hours, it was 40min to stir bleaching time in decolouring kettle, and other techniques are in the same manner as in Example 4, repeat no more.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 98.4%, steam
It is 8.5 hours to evaporate the time, supplies consumption 0.9%.
Embodiment 8：
On the basis of embodiment 5-7,2, the 5- dimethyl-2,5- is double（Tert-butyl peroxide）Hexane purifying technique,
Also include filtering 2,5- dimethyl -2,5- pair after separating（Tert-butyl peroxide）Hexane is delivered to the first measuring tank 35, profit
It is with air compressor machine 27 that 2,5- dimethyl -2,5- is double（Tert-butyl peroxide）Hexane is delivered to high-order measuring tank 30, by the first mistake
The filter filtering of device 34 stores into finished product storage device 33 to be produced；Or filtered successively by the first filter 34, the second metering
The metering storage of tank 31, the second filter 32 filters, and eventually enters into finished product storage device 33 and stores and produces.
2,5- dimethyl -2,5- that embodiment purification obtains is double（Tert-butyl peroxide）Hexane, purity 97.8%, steam
It is 8 hours to evaporate the time, supplies consumption 0.9%.
Test result indicates that any described purifying technique of embodiment 5-8 of the present invention, the institute of embodiment 1-4
Any purification system stated, the vacuum distillation time foreshortens to is reduced to less than 1.5% no more than 8.5h, target substance loss, target
Material purity is more than 97.5%.
After constant temperature and pressure distillation terminates, the present invention decolourizes obtained target product through decolouring kettle, and product color is bright, logical
Thoroughly, quality is high, meets company standard and Customer Quality requirement.
2 tons of 2,5- dimethyl -2,5- bis(t-butylperoxy) hexanes are produced by daily, vacuum distillation 5 times daily, every time
Distillation can reduce product and be lost 20 kilograms after employing new technology, add up to 100 kilograms.By the 80 yuan of calculating of market price per kilogram, this hair
The economic benefit that the purification process of bright offer is brought daily is 8000 yuan, and whole year is by 800 tons of production, caused direct economic benefit
At 6,400,000 yuan or so.Another to add the expense such as the electricity saved, water, artificial, whole year amounts to caused economic benefit probably 7,000,000
Member or so.
In addition, 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane purity bring up to 97.5% from 95%, quality
Raising can strengthen product competitiveness in the market, and sale value can improve 5000 yuan/ton.
Comparing embodiment：
By 2,5- dimethyl -2,5- pair that 600 kilograms of purity are 80%（Tert-butyl peroxide）Hexane crude product loads 1000L
In distillation still, distillation still chuck water bath heating system is opened, and automatic constant-temperature is at 40 DEG C；Then vacuum pump assembly is started, to kettle
Inside depressurized, when being shown in -0.095MPa to vacuum meter in kettle.After being evaporated under reduced pressure 14h, stop heating, the material that will be obtained
With activated carbon decolorizing, filter off except mechanical admixture, it is double to obtain 2,5- dimethyl -2,5-（Tert-butyl peroxide）Hexane, described 2,
5- dimethyl -2,5- is double（Tert-butyl peroxide）The purity of hexane is 91%, is lost as 7%.
Above-described embodiment, the purpose of the present invention, technical scheme and beneficial effect are carried out further
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., all should include
Within protection scope of the present invention.
Claims (7)
1. one kind 2, the purifying plant of double (tert-butyl peroxide) hexanes of 5- dimethyl -2,5-, it is characterised in that：Including distillation still
(21), decolouring kettle (22)；Distillation still (21) is connected by feeding pipe with decolouring kettle (22)；Distillation still (21) includes housing
(13), it is provided with that into blank pipe (6), to enter one end of blank pipe (6) with the distance from bottom of housing (13) be 10~200mm in housing (13),
The other end for entering blank pipe (6) is connected with the roof of housing (13)；
The purification system also includes destilling tower (23), condenser (24), collecting tank (25), and the roof of distillation still (21), which is provided with, to be steamed
Vapor outlet, steam (vapor) outlet are connected by conveyance conduit with the bottom inlet of destilling tower (23), and the top exit of destilling tower (23) leads to
Cross gas transmission pipeline to be connected with condenser (24), condenser (24) is connected with collecting tank (25), and collecting tank (25) collects condensation
Impurity and moisture mixed waste liquor out, condenser (24), collecting tank (25) are connected with Roots vaccum pump (29)；
The purification system also includes the first measuring tank (35), the first filter (34), the second measuring tank (31), the second filtering
Device (32), finished product storage device (33), the outlet at bottom of the top entry of high-order measuring tank (30) and the first measuring tank (35)
Connection, high-order measuring tank (30) successively with the first filter (34), the second measuring tank (31), the second filter (32), into
Product storage device (33) connects, and the first measuring tank (35) is connected to air compressor machine (27) and vavuum pump (28)；
It is described enter blank pipe (6) other end end be provided with needle valve (7), it is described enter blank pipe (6) number be 2~4, and in shell
It is uniformly and symmetrically distributed in body (13) using the central shaft of distillation still (21) as axle, the outlet at bottom of the decolouring kettle (22) passes through conveying
Pipeline is connected with Suction filtration device (26).
2. a kind of purifying plant of double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- according to claim 1, its
It is characterised by：The top of the decolouring kettle (22) is provided with activated carbon charging device.
3. a kind of purifying plant of double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- according to claim 1, its
It is characterised by：Gas-adding pipe (10) with being connected inside housing (13) is installed on the roof of the housing (13).
4. one kind is used for double (the peroxidating uncles of 2,5- dimethyl-2,5- using purifying plant described in claim 1-3 any one
Butyl) hexane purifying technique, it is characterised in that：Double (tert-butyl peroxide) the hexane semi-finished product of 2,5- dimethyl -2,5- are inhaled
Enter in distillation still (21), heating distillation still (21) to 61 DEG C~68 DEG C of temperature in the kettle, constant temperature；
In heating process, it is in negative pressure to make in distillation still, opens needle valve (7), is passed through air, the double (peroxides of 2,5- dimethyl -2,5-
Change the tert-butyl group) hexane be in fluidized state under air effect power, start to distill, to sampling analysis product design it is qualified after stop steaming
Evaporate；
By the interior product press-in decolouring kettle (22) of distillation still (21), decolorising agent, stirring, to sampling analysis are added to decolouring kettle (22) is interior
Product 2, double (tert-butyl peroxide) the hexane colourities of 5- dimethyl -2,5- are qualified, produce.
5. a kind of purifying technique of double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- according to claim 4, its
It is characterised by：In the heating process, vacuum is -0.093MPa~-0.098MPa in distillation still；The distillation time is
7.5~8.5 hours.
6. a kind of purifying technique of double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- according to claim 5, its
It is characterised by：The mixing time is 20~40 minutes.
7. the purification work of double (tert-butyl peroxide) hexanes of 2,5- of one kind dimethyl -2,5- according to claim 5 or 6
Skill, it is characterised in that：Double (tert-butyl peroxide) the hexane volumes of 2,5- dimethyl -2,5- are distillation still in the addition distillation still
The 50~65% of volume.
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| CN104910058B (en) * | 2015-04-20 | 2018-08-17 | 四川宜宾恒德化学有限公司 | A kind of 2,5- dimethyl -2,5- is double（T-butylperoxy）The purification process of hexane |
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