CN106608797A - Separation method for material flow containing 2,6-DIPN - Google Patents
Separation method for material flow containing 2,6-DIPN Download PDFInfo
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- CN106608797A CN106608797A CN201510685836.4A CN201510685836A CN106608797A CN 106608797 A CN106608797 A CN 106608797A CN 201510685836 A CN201510685836 A CN 201510685836A CN 106608797 A CN106608797 A CN 106608797A
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Abstract
The invention relates to a separation method for a material flow containing 2,6-DIPN, and mainly solves the technical problems in the prior art that product purity is low and energy consumption is high during separation and purification of 2,6-DIPN. The technical scheme of the invention is characterized in that the separation method comprises the following steps: mixed material liquid containing the 2,6-DIPN is deprived of light and heavy components through a wall-dividing rectifying tower, and then enters a first crystallizer to obtain a material flow containing coarse 2,6-DIPN through a suspension crystallization process; and coarse crystals enter a second crystallizer to obtain a high-purity 2,6-DIPN product through solvent crystallization, washing and drying processes, so that the above technical problems are well solved, and the separation method can be applied to industrial production of separation and purification of the 2,6-DIPN.
Description
Technical field
The present invention relates to a kind of separation method containing 2,6-DIPN logistics, can be used for separating-purifying 2,6-DIPN
Commercial production in.
Background technology
2,6-DIPN (2,6-DIPN) is a kind of important Organic Chemicals, oxidized generation NDA,
The latter can be used to prepare various high-performance polymers, the PEN that the esterification of itself and ethylene glycol, polycondensation are obtained
(PEN), because the rigidity of naphthalene nucleus in molecular structure is more than phenyl ring, therefore, compare poly terephthalic acid second general at present
Diol ester (PET), PEN has higher physical and mechanical propertiess, gas barrier property, chemical stability and heat-resisting, resistance to
The performances such as ultraviolet, radiation hardness, can be processed into thin film, fiber, hollow container and sheet material etc., before having a wide range of applications
Scape.
2,6-DIPN are mainly generated by naphthalene with propylene or isopropanol reaction, in the product of naphthalene and propylene isopropylation,
Outside 2,6-DIPN, also containing single isopropyl naphthalene (MIPN), the isomerss (DIPN) of other diisopropyl naphthalenes, three
Isopropyl naphthalene (TIPN), many isopropyl naphthalenes (PIPN), and the naphthalene that unreacted is complete.Because impurity is more in product,
And the isomerss of the diisopropyl naphthalene up to content of 10, especially 2,7-DIPN is suitable with the content of 2,6-DIPN,
Cause the product purity of 2,6-DIPN relatively low, and when being used to synthesize NDA, its purity requirement in terms of mass fraction
95% is not less than, accordingly, it would be desirable to carry out above-mentioned product separating-purifying just to can be used to synthesize NDA, and then
Prepare PEN.
In above-mentioned product, due to diisopropyl naphthalene and naphthalene, single isopropyl naphthalene, between triisopropyl naphthalene and many isopropyl naphthalenes
Boiling point has differences, and the method for simple rectification can be adopted to be separated, and obtains the mixture of diisopropyl naphthalene, but product
The isomerss species of middle diisopropyl naphthalene is more, and boiling point is also very close, between 308.6～319.6 DEG C, especially
2,7-DIPN, it is differed only by with the boiling point of 2,6-DIPN less than 2 DEG C (the former is 317 DEG C, and the latter is 319.6 DEG C), in addition
It is suitable with the content of 2,6-DIPN, it is clear that using the method for conventional rectification be cannot to obtain high-purity 2,6-DIPN products,
Therefore, in the method for separating-purifying 2,6-DIPN, the separation of diisopropyl naphthalene isomerss is key, especially
It is that 2,6-DIPN is separated with 2,7-DIPN.
At present the method for separating-purifying 2,6-DIPN mainly includes rectification method, crystallization process, complexation-crystallization method, absorption method,
And their combined methods each other：
Variant with the boiling point of other components based on diisopropyl naphthalene, CN1112539 proposes a kind of isopropyl naphthalene mixture
Three tower batch rectification methods, but it mainly carries out the cutting of above-mentioned fraction, by other diisopropyl naphthalene isomerss boiling points
Close impact, it is impossible to directly obtain 2,6-DIPN products, and multitower lock out operation brings remixing for intermediate species,
Cause the high energy consumption of distillation process.
Fusing point based on diisopropyl naphthalene isomerss is variant, except the fusing point of 2,6-DIPN higher (67～70 DEG C) outward,
The fusing point of other diisopropyl naphthalene isomerss is relatively low, and especially the fusing point of 2,7-DIPN is only -3 DEG C,
CN1793088A proposes naphthalene can be faced into hydrogen isopropyl by the method for vacuum distillation and first stage suspension crystallization plus the crystallization of one-level laminar
2,6-DIPN in glycosylation reaction product is separated, but it does not limit the operating condition of explanation vacuum distillation, and two steps yet
The temperature of crystallization process is all than relatively low (- 20 DEG C or so), in addition, 2, the 6-DIPN products in order to obtain purity >=99%, need
Multiple laminar crystallization is carried out, technique and operation are relative complex.
Variant based on diisopropyl naphthalene isomerss dissolubility in a solvent, CN101130478A proposes naphthalene and propylene
Product 2, the 6-DIPN products that purity is 99.0～99.5% can be obtained by the method for vacuum distillation and solvent crystallization,
But it does not limit the operating condition of explanation vacuum distillation, including number, number of theoretical plate, operating pressure, the reflux ratio of rectifying column
Deng, and the method only with solvent crystallization separates 2,6-DIPN and 2,7-DIPN, and not only the time of crystallization process is very long
(20～36 hours), and need to carry out single-stage or multistage recrystallization, cause the consumption of solvent very big.
Complex can be formed with other compounds based on 2,6-DIPN, and easily crystalline deposit is separated out, US4962274 is carried
Go out with 9,9 '-two anthracenes for chelating agent, with acetone as solvent, by the complex of reaction 2,6-DIPN of production, complex crystallization
After precipitation, then Jing is filtered, washed, being dried, the method that heating under reduced pressure decomposes can obtain the 2,6-DIPN of purity 99.8%, but its
Operation is more, and flow process is relative complex, and condition during heating under reduced pressure harsher (200 DEG C of pressure 25mmHg, temperature),
It is unfavorable for industrial amplification.
It is different from adsorbent surface inter-molecular binding force based on diisopropyl naphthalene isomerss, US4929796,
US5012039 and CN 101130481A propose to separate 2,6-DIPN and 2,7-DIPN, but product using the method for absorption
Purity not high (80.1～93.2%), it is still necessary to further to separate；US4992622 and US4950824 is it is also proposed that using suction
Attached method is capable of achieving the separating-purifying of 2,6-DIPN, although its product purity and yield are of a relatively high, in general
Absorbing process is more complicated, and the selectivity of adsorbent, adsorption capacity and desorption process all limit the effect of absorbing process,
There is not cost-effective adsorbent yet at present, constrain its industry and amplify.
Therefore, the purification technique of effective 2,6-DIPN is developed for the development for promoting China's polyester industrial has
Highly important meaning.More meaningful, due to rich coal resources in China, the separation for developing 2,6-DIPN is carried
Pure technology, is beneficial to make full use of the naphthalene in China's coal tar, is the high-purity 2,6-DIPN of raw material production with it,
And then raw material is provided to produce PEN, so as to greatly improve the utilization rate of resource.
The content of the invention
Flow process when being prior art separating-purifying 2,6- diisopropyl naphthalenes to be solved by this invention is complicated, product purity is low, energy
Consumption is high, be difficult the technical problem of industrial applications.There is provided a kind of method of new separating-purifying 2,6-DIPN, should
Method has the advantages that flow process is simple, product purity is high, energy consumption is low, is easy to amplify.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is as follows：Mixed liquor containing 2,6- diisopropyl naphthalenes
I enters rectifying tower with bulkhead, separated, and tower top obtains stream I I containing naphthalene, single isopropyl naphthalene, and side line is obtained containing diisopropyl
Stream I II of naphthalene, tower reactor obtains naphthalene containing triisopropyl and stream I V of other heavy constituents；Stream I II enters the first crystallizer,
Jing suspension crystallization processes obtain logistics V containing thick 2,6- diisopropyl naphthalenes crystal and logistics VI containing first degree crystalline mother solution；Thing
Stream V enters the second crystallizer, and with the solvent stream VII for adding, Jing solvent crystallizations, washing and dry run are obtained containing high-purity
Logistics VIII and stream I X containing secondary crystallization mother solution of 2,6- diisopropyl naphthalene products.
In above-mentioned technical proposal, 2,6-DIPN content by weight percentage is in preferred mixed liquor I
10～35%, in major impurity naphthalene content by weight percentage be 3～20%, 2,7- diisopropyl naphthalenes by weight percentage
Content be 10～40%.
In above-mentioned technical proposal, the demarcation strip of preferred rectifying tower with bulkhead is disposed vertically, and rectifying tower with bulkhead is divided on demarcation strip
The public rectifying section in portion, the public stripping section of demarcation strip bottom, and demarcation strip be located bulkhead section, bulkhead section be divided into again into
Material side and product side.
In above-mentioned technical proposal, the number of theoretical plate of preferred rectifying tower with bulkhead is no less than 30 pieces, wherein the theoretical plate of bulkhead section
Number is no less than 10 pieces, and the number of theoretical plate of public rectifying section is no less than 10 pieces, and the number of theoretical plate of public stripping section is no less than 10
Block.
In above-mentioned technical proposal, the number of theoretical plate of preferred rectifying tower with bulkhead is 30～60 pieces, wherein the theoretical plate of bulkhead section
Number is 10～20 pieces, and the number of theoretical plate of public rectifying section is 10～20 pieces, 10～20 pieces of the number of theoretical plate of public stripping section；
Mixed liquor I is entered from the feed side of bulkhead section, and charging aperture is located at the 4th～10 piece of theoretical plate from demarcation strip top down number；
Stream I II is produced from the product side of bulkhead section, produces mouth positioned at the 6th～20 piece of theoretical plate from demarcation strip top down number.
In above-mentioned technical proposal, the operating pressure that preferred rectifying tower with bulkhead is counted with absolute pressure as 5～30KPa, reflux ratio be 0.5～
4.0th, the liquid phase of public rectifying section enters bulkhead section feeding side and the liquid phase distribution ratio with molar percent of product side is
0.1～0.8, the gas phase of public stripping section enters the gas phase distribution ratio with molar percent of bulkhead section feeding side and product side
For 1.8～3.8.
In above-mentioned technical proposal, the first crystallizer uses suspension crystallization process, and preferred crystallization temperature is -20～10 DEG C.
In above-mentioned technical proposal, the second crystallizer uses solvent crystallization process, and preferred crystallization temperature is 0～25 DEG C.
In above-mentioned technical proposal, preferred solvent is alcohol compound, including ethanol, propanol, isobutanol etc., and solvent is tied
Solvent used by brilliant and washing process can be with identical or differ.
As it was previously stated, in the product of naphthalene and propylene isopropylation, being close to 2,6-DIPN boiling point containing more
Diisopropyl naphthalene isomerss, directly high-purity 2,6-DIPN product cannot be obtained using the method for rectification, together
When, because the fusing point (80.1 DEG C) of naphthalene in product is higher than (67～70 DEG C) of the fusing point of 2,6-DIPN, directly adopt
Method with crystallization will separate out the crystal containing a large amount of naphthalenes, cannot also obtain high-purity 2,6-DIPN product.The present invention is adopted
The separating-purifying of 2,6-DIPN is carried out with the group technology of rectification-crystallization, i.e., first by removing using rectifying tower with bulkhead
Light, heavy constituent in raw material, not only avoid and during later crystallization first separate out naphthalene and not separate out 2,6-DIPN brilliant
Body；And the removing of heavy constituent had both improve the product content in the crystallization temperature and coarse-grain of later crystallization process, further improved
The colourity of crystal, improves the visuality of product quality and crystallization process；Meanwhile, the use of rectifying tower with bulkhead not only keeps away
That has exempted from intermediate species when traditional two towers separate three components remixes caused energy dissipation, and reduces a rectifying column
And a set of vaporization and condensation system, reduce occupation of land space and equipment investment；Subsequently, based on other diisopropyl naphthalene isomers
Boiling point is close with 2,6-DIPN, and fusing point but has many difference, is first separated out using the method for suspension crystallization and is rich in 2,6- bis-
The crystal of isopropyl naphthalene, realizes 2,6-DIPN and efficiently separating except the isomerss outside 2,7- diisopropyl naphthalenes,
The content of 2,7- diisopropyl naphthalenes in coarse-grain has been greatly reduced simultaneously；Then, based on alcohol compound, such as ethanol, propanol,
Isopropanol etc. has at different temperatures a notable difference to the dissolubility of 2,6-DIPN, and alcohols material polarity is relatively strong, boiling
Point is relatively low and cheap and easy to get, then with above-claimed cpd as solvent, using what the method for solvent crystallization realized product one is entered
Step purification, especially realizes efficiently separating for 2, the 7- diisopropyl naphthalene closest with boiling point, high-purity so as to obtain
2,6- diisopropyl naphthalene products.
From the comparison of embodiment and comparative example can be seen that for cut after light, heavy constituent containing 2,6-DIPN
For mixed liquor, during the method crystallized using first solvent crystallization settling flux, not only crystallization time is very long during solvent crystallization,
And also contain more 2,7- diisopropyl naphthalenes in the 2,6-DIPN product after separating, suspension crystallization is now passed through again
Method, it is impossible to effectively remove 2,7- diisopropyl naphthalenes therein, cause product purity low；Directly using solvent crystallization
During method, because impurity content is high, in order to improve product purity, it is necessary to carry out one or more levels recrystallization, need to consume more
Many solvents, while further increasing the time of solvent crystallization process；During using the first suspension crystallization method that again laminar is crystallized,
Although not using solvent, in order to improve product purity, it is also necessary to multistage low temperature laminar crystallization is carried out, however, due to impurity
Plane of crystal is easily attached on, the raising of product purity is limited, in addition laminar crystallization process is intermittently operated, is unfavorable for industry
Amplify.And using the method for first suspension crystallization solvent crystallization again in embodiment, not only crystallization time is short, solvent load is few, and
And process is simple, product purity are higher；In addition substitute traditional two towers separation cutting diisopropyl naphthalene using rectifying tower with bulkhead to mix
Closing feed liquid energy consumption substantially reduces, therefore, can more preferable separating-purifying using rectification of the present invention-crystallization combined method
2,6-DIPN, and reducing energy consumption.
Using technical scheme, light, the heavy constituent in rectifying tower with bulkhead removing diisopropyl naphthalene mixed liquor is first passed through,
Again by the compound mode of first suspension crystallization solvent crystallization again, both reduced the energy consumption of distillation process, in turn ensure that product purity,
Product quality is improve, and while solvent load is reduced, is also improved crystallization temperature and is shortened crystallization process
Time.Compared with prior art, the present invention has that flow process is simple, product purity can improve more than 2.5%, rectifying tower with bulkhead
Energy consumption more common two tower rectification can reduce by more than 15% advantage, achieve good technique effect.
Description of the drawings
Fig. 1 is the separating technology flow chart of the logistics of diisopropyl naphthalene containing 2,6- involved in the present invention
Fig. 2,3,4 are the separating technology flow chart of the logistics of diisopropyl naphthalene containing 2,6-
Fig. 5 is the process chart that the logistics of diisopropyl naphthalene containing 2,6- is separated using common rectifying tower
In Fig. 1, D1 be rectifying tower with bulkhead, C1 be the first crystallizer of suspension crystallization process, C2 be solvent crystallization process
The second crystallizer.It is containing naphthalene, Dan Yi that logistics (101) is the mixed liquor containing 2,6- diisopropyl naphthalenes, logistics (102)
The rectifying tower with bulkhead overhead of propyl group naphthalene, logistics (103) be the rectifying tower with bulkhead side stream containing diisopropyl naphthalene,
Logistics (104) be the rectifying tower with bulkhead tower reactor distillation of naphthalene containing triisopropyl and other heavy constituents, logistics (105) be through
The magma rich in 2,6- diisopropyl naphthalenes, logistics (106) after crystallizer C1 separation is after crystallizer C1 is separated
First degree crystalline mother solution rich in other diisopropyl naphthalene isomerss, logistics (107) for solvent crystallization process add it is molten
Agent, logistics (108) are 2,6- diisopropyl naphthalene products, the logistics (109) after the further separating-purifyings of crystallizer C2
It is the rich solvent-laden secondary crystallization mother solution after crystallizer C2 is separated.
In Fig. 2, D1 is still rectifying tower with bulkhead, E1 is the first crystallizer of solvent crystallization process, E2 is suspension crystallization mistake
Second crystallizer of journey.Logistics (201)～logistics (204) is with the logistics (101) in Fig. 1～logistics (104), logistics
(205) it is rich in 2,6- after crystallizer E1 is separated for the solvent of addition, logistics (206) during solvent crystallization
The magma of diisopropyl naphthalene, logistics (207) are rich solvent-laden first degree crystalline mother solution, the thing after crystallizer E1 is separated
It is Jing that stream (208) is 2,6- diisopropyl naphthalene products after the further separating-purifyings of crystallizer E2, logistics (209)
The secondary crystallization mother solution containing other diisopropyl naphthalene isomerss crossed after crystallizer E2 is separated.
In Fig. 3, D1 is still rectifying tower with bulkhead, F1 is the first crystallizer of solvent crystallization process, F2 is solvent recrystallization
Second crystallizer of process.Logistics (301)～logistics (307) is with the logistics (201) in Fig. 2～logistics (207), thing
It is through weight that stream (308) is 2,6- diisopropyl naphthalene products after the further separating-purifying of recrystallization, logistics (309)
The secondary crystallization mother solution rich in solvent He other diisopropyl naphthalene isomerss after Crystallization Separation.
In Fig. 4, D1 is still rectifying tower with bulkhead, G1 is the first crystallizer of suspension crystallization process, G2 was crystallized for laminar
Second crystallizer of journey.Logistics (401)～logistics (406) is with the logistics (101) in Fig. 1～logistics (106), logistics
(407) be 2,6- diisopropyl naphthalene products after the further separating-purifyings of crystallizer G2, logistics (408) be through
The secondary crystallization mother solution containing other diisopropyl naphthalene isomerss after crystallizer G2 separation.
In Fig. 5, B1 is the first rectifying column for cutting light component, Second distillation column, C1, C2 that B2 is cutting heavy constituent
Same Fig. 1.It is containing naphthalene, single isopropyl naphthalene that logistics (501) is the mixed liquor containing 2,6- diisopropyl naphthalenes, logistics (502)
The overhead of rectifying column B1, logistics (503) be the essence containing diisopropyl naphthalene, triisopropyl naphthalene and other heavy constituents
It is the overhead of the rectifying column B2 containing diisopropyl naphthalene, logistics (505) to evaporate the tower reactor distillation of tower B1, logistics (504)
Tower reactor distillation, the logistics (506) for being naphthalene containing triisopropyl and the rectifying column B2 of other heavy constituents is through crystallizer C1
The magma rich in 2,6- diisopropyl naphthalenes, logistics (507) after separation be through crystallizer C1 separate after rich in other two
Solvent, logistics (509) that the first degree crystalline mother solution of isopropyl naphthalene isomerss, logistics (508) are added for solvent crystallization process
Be 2,6- diisopropyl naphthalene products after the further separating-purifyings of crystallizer C2, logistics (510) be through crystallizer
Rich solvent-laden secondary crystallization mother solution after C2 separation.
Below by embodiment, the invention will be further elaborated.
Specific embodiment
【Embodiment 1】
Using the flow process shown in Fig. 1, logistics (101) is the mixed liquor containing 2,6-DIPN, feed rate 1Kg/hr,
Consisting of with weight percentage：Naphthalene 19.28%, single isopropyl naphthalene 49.03%, 2,6- diisopropyl naphthalenes 10.77%, 2,7-
The heavy constituents 4.23% such as diisopropyl naphthalene 16.69%, other diisopropyl naphthalenes and triisopropyl naphthalene.
The number of theoretical plate of rectifying tower with bulkhead D1 is 60, and wherein the number of theoretical plate of bulkhead section is 20, the theoretical plate of public rectifying section
Number is 20, the number of theoretical plate 20 of public stripping section, and logistics (101) is managed from the 8th piece of rectifying tower with bulkhead bulkhead section feeding side
Enter by plate, logistics (103) is produced from the 10th piece of theoretical plate of rectifying tower with bulkhead bulkhead section product side, and operating pressure is
10KPa, reflux ratio is 0.75, the liquid phase of public rectifying section enter bulkhead section feeding side and product side with molar percent
Liquid phase distribution ratio be 0.50, the gas phase of public stripping section enter bulkhead section feeding side and product side with molar percent
Gas phase distribution ratio is 3.44, and the energy consumption of rectifying tower with bulkhead is 0.26KW；2,6- diisopropyl naphthalenes in logistics (103) after separation
By weight percentage consist of 39.98%；Into crystallizer C1, crystallization temperature is -10 DEG C, crystallization for logistics (103)
Time is 5hr, and Jing suspension crystallization and after filtering, 2,6-DIPN is by weight percentage in the crystal of logistics (105)
Purity be 83.61%；Logistics (105) goes successively to crystallizer C2, and solvent is ethanol, and crystallization temperature is 8 DEG C, crystallization
Time is 5.5hr, after Jing solvent crystallizations, washing with alcohol, and filtration, drying, 2,6- bis- in the product of logistics (108)
Isopropyl naphthalene purity by weight percentage is 99.75%, and wherein solvent and the mass ratio of raw material are 1.02:1.
【Embodiment 2】
Constituted using flow process same as Example 1 and raw material.The number of theoretical plate of rectifying tower with bulkhead D1 is 45, wherein bulkhead
The number of theoretical plate of section is 15, and the number of theoretical plate of public rectifying section is 15, the number of theoretical plate 15 of public stripping section, logistics (101)
Enter from the 4th piece of theoretical plate of rectifying tower with bulkhead bulkhead section feeding side, logistics (103) is from rectifying tower with bulkhead bulkhead section product
The 10th piece of theoretical plate extraction of side, operating pressure is 20KPa, and reflux ratio is 1.0, and the liquid phase of public rectifying section enters bulkhead
As 0.14, the gas phase of public stripping section enters bulkhead section to the liquid phase distribution ratio with molar percent of section feeding side and product side
As 2.14, the energy consumption of rectifying tower with bulkhead is 0.31KW to the gas phase distribution ratio with molar percent of feed side and product side；
After separation in logistics (103) 2,6- diisopropyl naphthalenes by weight percentage consist of 39.98%；Logistics (103) is entered
Crystallizer C1, crystallization temperature is -15 DEG C, and crystallization time is 6hr, Jing suspension crystallization and after filtration, the crystalline substance of logistics (105)
2,6- diisopropyl naphthalenes purity by weight percentage is 81.84% in body；Logistics (105) goes successively to crystallizer C2,
Solvent is ethanol, and crystallization temperature is 5 DEG C, and crystallization time is 6hr, and Jing solvent crystallizations, methanol are washed, and filters, does
After dry, 2,6-DIPN purity by weight percentage is 99.71% in the product of logistics (108), wherein solvent
It is 0.96 with the mass ratio of raw material:1.
【Embodiment 3】
Using the flow process shown in Fig. 1, logistics (101) is the mixed liquor containing 2,6-DIPN, feed rate 1Kg/hr,
Consisting of with weight percentage：Naphthalene 11.39%, single isopropyl naphthalene 31.53%, 2,6- diisopropyl naphthalenes 20.18%, 2,7-
The heavy constituents 6.29% such as diisopropyl naphthalene 30.61%, other diisopropyl naphthalenes and triisopropyl naphthalene.
The number of theoretical plate of rectifying tower with bulkhead D1 is 30, and wherein the number of theoretical plate of bulkhead section is 10, the theoretical plate of public rectifying section
Number is 10, the number of theoretical plate 10 of public stripping section, and logistics (101) is managed from the 4th piece of rectifying tower with bulkhead bulkhead section feeding side
Enter by plate, logistics (103) is produced from the 8th piece of theoretical plate of rectifying tower with bulkhead bulkhead section product side, and operating pressure is 5KPa,
Reflux ratio is 1.6, and the liquid phase of public rectifying section enters the liquid phase with molar percent point of bulkhead section feeding side and product side
Proportioning is 0.57, and the gas phase of public stripping section enters the gas phase distribution with molar percent of bulkhead section feeding side and product side
It is 0.26KW than the energy consumption for 2.94, rectifying tower with bulkhead；After separation in logistics (103) 2,6- diisopropyl naphthalenes with weight hundred
Divide and consist of 40.24% than meter；Logistics (103) is -5 DEG C into crystallizer C1, crystallization temperature, and crystallization time is 4hr,
Jing suspension crystallization and after filtration, 2,6-DIPN purity by weight percentage is in the crystal of logistics (105)
87.63%；Logistics (105) goes successively to crystallizer C2, and solvent is propanol, and crystallization temperature is 12 DEG C, and crystallization time is
After 4.5hr, Jing solvent crystallization, washing with alcohol, and filtration, drying, 2,6- diisopropyls in the product of logistics (108)
Naphthalene purity by weight percentage is 99.79%, and wherein solvent and the mass ratio of raw material are 2:1.
【Embodiment 4】
Constituted using flow process same as Example 3 and raw material.The number of theoretical plate of rectifying tower with bulkhead D1 is 60, wherein bulkhead
The number of theoretical plate of section is 20, and the number of theoretical plate of public rectifying section is 20, the number of theoretical plate 20 of public stripping section, logistics (101)
Enter from the 6th piece of theoretical plate of rectifying tower with bulkhead bulkhead section feeding side, logistics (103) is from rectifying tower with bulkhead bulkhead section product
The 18th piece of theoretical plate extraction of side, operating pressure is 30KPa, and reflux ratio is 1.2, and the liquid phase of public rectifying section enters bulkhead
As 0.19, the gas phase of public stripping section enters bulkhead section to the liquid phase distribution ratio with molar percent of section feeding side and product side
As 3.09, the energy consumption of rectifying tower with bulkhead is 0.24KW to the gas phase distribution ratio with molar percent of feed side and product side；
After separation in logistics (103) 2,6- diisopropyl naphthalenes by weight percentage consist of 40.24%；Logistics (103) is entered
Crystallizer C1, crystallization temperature is -10 DEG C, and crystallization time is 5hr, Jing suspension crystallization and after filtration, the crystalline substance of logistics (105)
2,6- diisopropyl naphthalenes purity by weight percentage is 85.98% in body；Logistics (105) goes successively to crystallizer C2,
Solvent is isopropanol, and crystallization temperature is 10 DEG C, and crystallization time is 5hr, and Jing solvent crystallizations, isopropanol are washed, and filter,
After drying, 2,6-DIPN purity by weight percentage is 99.77% in the product of logistics (108), wherein molten
Agent is 1.87 with the mass ratio of raw material:1.
【Embodiment 5】
Using the flow process shown in Fig. 1, logistics (101) is the mixed liquor containing 2,6-DIPN, with weight percentage
Consist of：Naphthalene 5.06%, single isopropyl naphthalene 13.14%, 2,6- diisopropyl naphthalenes 34.71%, 2,7- diisopropyl naphthalenes 37.49%,
The heavy constituent such as other diisopropyl naphthalenes and triisopropyl naphthalene 9.60%.
The number of theoretical plate of rectifying tower with bulkhead D1 is 60, and wherein the number of theoretical plate of bulkhead section is 20, the theoretical plate of public rectifying section
Number is 20, the number of theoretical plate 20 of public stripping section, the 10th piece from rectifying tower with bulkhead bulkhead section feeding side of logistics (101)
Theoretical plate is entered, and logistics (103) is produced from the 15th piece of theoretical plate of rectifying tower with bulkhead bulkhead section product side, and operating pressure is
15KPa, reflux ratio is 3.5, the liquid phase of public rectifying section enter bulkhead section feeding side and product side with molar percent
Liquid phase distribution ratio is 0.15, and the gas phase of public stripping section enters the gas with molar percent of bulkhead section feeding side and product side
Phase partitioning ratio is 3.58, and the energy consumption of rectifying tower with bulkhead is 0.39KW；After separation in logistics (103) 2,6- diisopropyl naphthalenes with
Percentage by weight meter consists of 47.83%；Into crystallizer C1, crystallization temperature is 5 DEG C, crystallization time for logistics (103)
For 2.5hr, Jing suspension crystallization and after filtering, 2,6-DIPN is by weight percentage in the crystal of logistics (105)
Purity is 91.35%；Logistics (105) goes successively to crystallizer C2, and solvent is ethanol, and crystallization temperature is 20 DEG C, crystallization
Time is 3hr, and after Jing solvent crystallizations, washing with alcohol, and filtration, drying, 2,6- bis- is different in the product of logistics (108)
Propyl group naphthalene purity by weight percentage is 99.85%, and wherein solvent and the mass ratio of raw material are 3.79:1.
【Comparative example 1】
Using the flow process shown in Fig. 2, constituted using raw material same as Example 1, the operating condition of rectifying tower with bulkhead D1
With embodiment 1, the logistics (203) after separation into crystallizer E1, logistics (205) for solvent crystallization process ethanol
Solvent, solvent is 1.1 with the mass ratio of raw material:1, crystallization temperature is 30 DEG C, and crystallization time is 36 hours, and Jing is filtered, second
Repeatedly after washing, 2,6-DIPN purity by weight percentage is 90.16% to alcohol in the crystal of logistics (206),
Wherein 2,7- diisopropyl naphthalenes content by weight percentage is 8.33%；Logistics (206) goes successively to crystallizer E2,
Crystallization temperature is 45 DEG C, and crystallization time is 5hr, Jing suspension crystallization, after filtering and being dried, in the product of logistics (208)
2,6-DIPN purity by weight percentage is 93.24%, wherein 2,7- diisopropyl naphthalenes are by weight percentage
Content is 6.23%.
【Comparative example 2】
Using the flow process shown in Fig. 3, constituted using raw material same as Example 1, rectifying tower with bulkhead D1 and crystallizer F1
Operating condition with the rectifying tower with bulkhead D1 and crystallizer E1 in comparative example 1, the logistics (306) after separation goes successively to
Crystallizer F2 carries out recrystallization, and crystallization temperature is 45 DEG C, and crystallization time is 20hr, Jing recrystallization, after filtering and being dried,
2,6-DIPN purity by weight percentage is 97.21% in the product of logistics (308), wherein 2,7- diisopropyls
Base naphthalene content by weight percentage is 2.48%, and total solvent load and the mass ratio of raw material is 2.56:1.
【Comparative example 3】
Using the flow process shown in Fig. 4, constituted using raw material same as Example 1, rectifying tower with bulkhead D1 and crystallizer G1
Operating condition with the rectifying tower with bulkhead D1 and crystallizer C1 in embodiment 1, the logistics (405) after separation goes successively to
Crystallizer G2 carries out laminar crystallization, and crystallization temperature is 45 DEG C, and crystallization time is 4hr, after crystallized, diaphoresis, logistics (407)
Product in 2,6-DIPN purity by weight percentage be 94.88%, wherein 2,7- diisopropyl naphthalenes are with weight hundred
It is 4.92% to divide than the content of meter.
【Comparative example 4】
Using the flow process shown in Fig. 5, adopt and constituted with embodiment 1, the identical raw material of embodiment 2, the reason of rectifying column B1
It is 30 by plate number, logistics (501) is entered from the 20th piece of theoretical plate, and operating pressure is 10KPa, and reflux ratio is 0.5；Essence
The number of theoretical plate for evaporating tower B2 is 30, and logistics (503) is entered from the 20th piece of theoretical plate, and operating pressure is 10KPa, backflow
Than for 0.5；After separation in logistics (504) 2,6- diisopropyl naphthalenes by weight percentage consist of 39.98%；Crystallized
The condition of journey is 0.34KW with embodiment 1, the now energy consumption of rectifying column B1, and the energy consumption of rectifying column B2 is 0.07KW,
Therefore, compared with two traditional tower rectification process, the rectifying tower with bulkhead energy consumption in embodiment 1 saves 36.59% compared with it, in fact
The rectifying tower with bulkhead energy consumption applied in example 2 saves 24.39% compared with it.
【Comparative example 5】
Using the flow process shown in Fig. 5, adopt and constituted with embodiment 3, the identical raw material of embodiment 4, the reason of rectifying column B1
It is 25 by plate number, logistics (501) is entered from the 17th piece of theoretical plate, and operating pressure is 5KPa, and reflux ratio is 0.9；Rectification
The number of theoretical plate of tower B2 is 25, and logistics (503) is entered from the 17th piece of theoretical plate, and operating pressure is 5KPa, reflux ratio
For 0.5；After separation in logistics (504) 2,6- diisopropyl naphthalenes by weight percentage consist of 40.24%；Crystallization process
Condition with embodiment 3, now the energy consumption of rectifying column B1 is 0.19KW, and the energy consumption of rectifying column B2 is 0.12KW, because
This, compared with two traditional tower rectification process, the rectifying tower with bulkhead energy consumption in embodiment 3 saves 16.13% compared with it, implements
Rectifying tower with bulkhead energy consumption in example 4 saves 22.58% compared with it.
Claims (9)
1. a kind of separation method containing 2,6-DIPN logistics, comprises the following steps：
A () contains 2, the mixed liquor I of 6- diisopropyl naphthalenes enters rectifying tower with bulkhead, separated, and tower top obtains stream I I containing naphthalene, single isopropyl naphthalene, side line obtains stream I II containing diisopropyl naphthalene, and tower reactor obtains naphthalene containing triisopropyl and stream I V of other heavy constituents；
B () above-mentioned stream I II enters the first crystallizer, Jing suspension crystallization processes obtain logistics V containing thick 2,6-DIPN crystal and logistics VI containing first degree crystalline mother solution；
C () above-mentioned logistics V enters the second crystallizer, with the solvent stream VII for adding, Jing solvent crystallizations, washing and dry run obtain logistics VIII containing high-purity 2,6-DIPN product and stream I X containing secondary crystallization mother solution.
2. it is according to claim 1 to contain 2, the separation method of 6- diisopropyl naphthalene logistics, it is characterized in that 2 in mixed liquor I, 6- diisopropyl naphthalenes content by weight percentage is 10～35%, naphthalene content by weight percentage is that 3～20%, 2,7- diisopropyl naphthalenes content by weight percentage is 10～40% in major impurity.
3. it is according to claim 1 to contain 2, the separation method of 6- diisopropyl naphthalene logistics, it is characterized in that the demarcation strip of rectifying tower with bulkhead is disposed vertically, rectifying tower with bulkhead is divided into into the public stripping section of the public rectifying section on demarcation strip top, demarcation strip bottom, and the bulkhead section that demarcation strip is located；Bulkhead section is divided into feed side and product side again.
4. it is according to claim 1 to contain 2, the separation method of 6- diisopropyl naphthalene logistics, it is characterized in that the number of theoretical plate of rectifying tower with bulkhead is no less than 30 pieces, wherein the number of theoretical plate of bulkhead section is no less than 10 pieces, the number of theoretical plate of public rectifying section is no less than 10 pieces, and the number of theoretical plate of public stripping section is no less than 10 pieces.
5. according to claim 1,3 containing 2, the separation method of 6- diisopropyl naphthalene logistics, it is characterized in that the number of theoretical plate of rectifying tower with bulkhead is 30～60 pieces, wherein the number of theoretical plate of bulkhead section is 10～20 pieces, the number of theoretical plate of public rectifying section is 10～20 pieces, 10～20 pieces of the number of theoretical plate of public stripping section；Mixed liquor I is entered from the feed side of bulkhead section, and charging aperture is located at the 4th～10 piece of theoretical plate from demarcation strip top down number；Stream I II containing diisopropyl naphthalene is produced from the product side of bulkhead section, produces mouth positioned at the 6th～20 piece of theoretical plate from demarcation strip top down number.
6. it is according to claim 1 to contain 2, the separation method of 6- diisopropyl naphthalene logistics, it is characterised in that rectifying tower with bulkhead enters the gas phase distribution ratio with molar percent of bulkhead section feeding side and product side as 1.8～3.8 with the liquid phase that the operating pressure that absolute pressure is counted is 5～30KPa, reflux ratio is 0.5～4.0, public rectifying section into the gas phase that the liquid phase distribution ratio with molar percent of bulkhead section feeding side and product side is 0.1～0.8, public stripping section.
7. the separation method containing 2,6-DIPN logistics according to claim 1, it is characterised in that suspension crystallization process is used in the first crystallizer, crystallization temperature is -20～10 DEG C.
8. the separation method containing 2,6-DIPN logistics according to claim 1, it is characterised in that solvent crystallization process is used in the second crystallizer, crystallization temperature is 0～25 DEG C.
9. the separation method containing 2,6-DIPN logistics according to claim 1, it is characterised in that solvent for use is alcohol compound, and solvent crystallization and the solvent used by washing process can be with identical or differ.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103319300A (en) * | 2013-07-05 | 2013-09-25 | 中国科学院大学 | Process method for preparing industrial naphthalene through continuous distillation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319300A (en) * | 2013-07-05 | 2013-09-25 | 中国科学院大学 | Process method for preparing industrial naphthalene through continuous distillation |
Non-Patent Citations (2)
| Title |
|---|
| 李文艳: "2,6-二异丙基萘分离精制方法的研究", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》 * |
| 马淑芬等: "2,6-二异丙基萘的合成与分离技术的进展", 《化学工业与工程》 * |
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