CN204281488U - A kind of cyclo-hexane oxidation waste alkali tripping device - Google Patents

A kind of cyclo-hexane oxidation waste alkali tripping device Download PDF

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CN204281488U
CN204281488U CN201420681600.4U CN201420681600U CN204281488U CN 204281488 U CN204281488 U CN 204281488U CN 201420681600 U CN201420681600 U CN 201420681600U CN 204281488 U CN204281488 U CN 204281488U
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separator
cyclo
waste
tripping device
waste alkali
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张晓辉
黄敬
余兴
王丹
胡璐
彭菲
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Abstract

The utility model discloses a kind of cyclo-hexane oxidation waste alkali tripping device, this device is composed in series successively by gravity separator, drop multiplication separator, cyclone separator and coalescing separator, this device is adopted effectively to be separated by the salkali waste in cyclohexane oxide solution, alkali and Organic Sodium Salt is prevented to be brought into alkane tower, when salkali waste separation system does not wash with water, effectively solve the halfway problem of prior art cyclohexane oxidation unit waste frying oil, process water 0.5 ~ 5m can be saved 3/ h, and the driving cycle of device can bring up to more than 12 months.

Description

A kind of cyclo-hexane oxidation waste alkali tripping device
Technical field
The utility model relates to a kind of cyclo-hexane oxidation waste alkali tripping device, belongs to cyclohexane oxidation Technology field.
Background technology
In process of cyclohexanone production, in the oxidation products that hexanaphthene and atmospheric oxidation are formed except hexalin, pimelinketone and cyclohexyl hydroperoxide, also containing other materials many, as ester, acid, aldehyde etc.; Process at decomposing pot internal oxidition liquid aqueous sodium hydroxide solution, decomposing cyclohexyl hydrogen peroxide generates pimelinketone, hexalin, acid is neutralized, and ester class then generates organic acid sodium salt and hexalin by saponification reaction, and a small amount of ketone, aldehyde condensation generate dipolymer and trimer; The waste lye obtained after having reacted enters salkali waste separation circuit, and be separated containing a small amount of pimelinketone, hexalin with alkali, water with the organic phase of a large amount of hexanaphthene composition, organic phase enters alkane distillation process.
Because oxidation products decomposes under alkaline environment, need to carry out settlement separate from decomposing hexanaphthene, degradation production, organic acid sodium salt and inorganic phase out.In the prior art, remove alkali in cyclohexane oxide solution, the method for water carries out natural separation according to the principle of gravity settling, in the organic phase after separation, still have the water of about 0.5%, alkali and Organic Sodium Salt.
In industrial flow design, by two to three separating tanks, two to three subgravities carry out to this strand of material settlement separate, but from the situation of many device actual motions, salkali waste separation system is separated bad always, salkali waste is dispersed in hexanaphthene with fine droplets, if these waste lyes are taken in follow-up alkane distillation tower with logistics, acyloin condensation is caused in hexanaphthene evaporator tower well heater, the reboiler fouling of alkane distillation tower can be caused, thus cause supplies consumption to increase, and the driving cycle of alkane distillation tower can significantly shorten, have a strong impact on normal production: when improving production load, after the liquid phase circulation amount of whole hexanaphthene system increases, the problem of hexanaphthene band alkali is more outstanding, larger impact is caused on the stably manufactured of whole device.
Gravity settling can realize being separated of hexanaphthene decomposed solution and waste lye, but separation efficiency is low, required time is long, facility investment is large, only have macrobead could sedimentation effectively, fine particle cannot sedimentation, solution by this method after separating treatment is obvious oyster white, and by gravity settling, oneself can not reach the object being thoroughly separated waste lye to these fine particles completely.The water droplet that gravity settling is only greater than 50 μm to particle diameter is effective.
For reducing the content of sodium ion in organic phase, secondary can be adopted to wash or multi-stage water wash.Organic phase is carried out in water washing process, the add-on of water should control 0.5 ~ 2.0wt% in hexanaphthene decomposed solution total amount, increase the add-on of water, be conducive to the dissolving of sodium salt, but do the consumption adding process water on the one hand like this, on the other hand because salkali waste need carry out evaporation and concentrating at subsequent processing, increase the water yield and certainly will increase steam consumption, feasibility is little economically.
Cyclonic separation is the density difference by immiscible organic phase and aqueous phase, tangentially enter separating cyclone tube, in separating cyclone tube, two-phase liquid at high speed rotates, produce centrifugal force, the centrifugal force born due to organic phase and aqueous phase differs greatly, thus organic phase is floated from tube hub, and aqueous phase sinks along inside pipe wall, achieve sharp separation under organic phase and aqueous phase hypergravity, thus reach the object efficiently purifying alkali in cyclohexane oxide solution, water.
But the water lotion after cyclonic separation is also containing micro-emulsified water, be separated necessary first breakdown of emulsion, after water lotion enters coalescing separator, successively by the breakdown of emulsion layer of the filtering layer in coalescing separator, glass fibre composition, the coalescing layer of organic synthetic fibers composition and stainless steel separating layer, make unsegregated small water droplet be agglomerated into large water droplet further, thus separate from organic phase.
Although the separation accuracy of coalescer is high, particle separation diameter can reach 0.1 μm, its exist liquid unholiness time easily cause element blocked shortcoming.Some strainer puts into operation, do not cross the high pressure drop that just there will be for several hours and be difficult to accept, and impact resistance is little, can lose separating power when alkali waste water content is larger.
Utility model content
For in prior art in the isolation technique of the waste lye in cyclohexane oxide solution, exist be separated thoroughly, the defect such as energy consumption is large, complicated operation; The purpose of this utility model is to provide a kind of device be separated that effectively can realize organic phase and waste lye in cyclohexane oxide solution, this device operating process is simple, can carry out continuously, energy consumption is low, meets the requirement except alkali waste water to cyclohexane oxide solution in industrial production.
The utility model discloses a kind of cyclo-hexane oxidation waste alkali tripping device, this cyclo-hexane oxidation waste alkali tripping device is composed in series by pipeline successively by gravity separator, drop multiplication separator, cyclone separator and coalescing separator.
Cyclo-hexane oxidation waste alkali tripping device of the present utility model also comprises following preferred version:
In preferred scheme, drop multiplication separator comprises original fluid container and separating tank; Rectifier, drop multiplication filler separation assembly and specific panel group formula phase separator assembly is provided with in described separating tank.
In preferred scheme, original fluid container, rectifier, drop multiplication filler separation assembly and specific panel group formula phase separator assembly set gradually from the raw material upstream end of drop multiplication separator to parting liquid output terminal.Original fluid container, rectifier, drop multiplication filler separation assembly and specific panel group formula phase separator assembly set gradually according to the trend of raw material to be separated in drop multiplication separator, raw material from original fluid container out, passes through rectifier, drop multiplication filler separation assembly and specific panel group formula phase separator assembly successively.
In preferred scheme, gravity separator adopts more than single-stage or two-stage to connect.Most preferably be two-stage gravity separator series combination.Gravity separator of the present utility model is the gravity separator of the various routines of the art.
In preferred scheme, coalescing separator adopts more than single-stage or two-stage to connect.The coalescing separator that the utility model is selected is the coalescing separator of this area routine.
The cyclone separator that the utility model is selected can be the cyclone separator of this area routine, or the cyclone separator adopting structure to simplify.The cyclone separator that structure simplifies comprises chamber and cyclone pipe, described chamber comprises feed cavity, oil phase outlet plenum and oily(waste)water outlet plenum, feed cavity, oil phase outlet plenum and oily(waste)water outlet plenum can be divided into three independent containers, or three parts in a container, to simplify the structure of production equipment; Described cyclone pipe shares feed cavity, oil phase outlet plenum and oily(waste)water outlet plenum three chambers.Most preferred cyclone separator structure, see Chinese patent ZL00217613.0.
Hinge structure, the utility model beneficial effect:
(a), gravity separator, drop multiplication separator, cyclone separator and coalescing separator perfect adaptation are become the device be separated of a set of waste lye that can effectively realize in cyclohexane oxide solution, cyclohexane oxide solution is by gravity settling technology, drop doubling technology, cyclone separation process and the process of Coalescence-separation Technology series combination, the relative merits of various technology are complementary, thus pass through more reasonably gradient distribution separation method, overcome the shortcoming that prior art cyclohexane oxidation solution salkali waste separating effect is undesirable.
B (), apparatus structure of the present utility model are simple, easy enforcement, easy to operate, can serialization produce, and be applicable to long-term operation, be applicable to the liquid-liquid separation that the devices such as oil-refining chemical are immiscible or solubleness is very low, be specially adapted to the separation to salkali waste in cyclohexane oxide solution, can again petroleum chemical industry be promoted the use of.
(c), the application of device of the present utility model in cyclohexane oxide solution in salkali waste separation, achieve and enter while sodium ion does not increase in alkane distillation tower material, reduce the usage quantity of salkali waste separation system process water, alleviate the processing load of salkali waste evaporization process, the cycle of operation of extension fixture.Process water 0.5 ~ 5m can be saved 3/ h, and the driving cycle of device can bring up to more than 12 months, save material consumption and energy consumption.
Accompanying drawing explanation
[Fig. 1] is cyclo-hexane oxidation waste alkali tripping device figure of the present utility model;
[Fig. 2] is the structure iron of drop multiplication separator;
The structure iron that [Fig. 3] is cyclone separator;
1 is gravity separator, and 2 is drop multiplication separator, and 3 is cyclone separator, 4 is coalescing separator, 5 is original fluid container, and 6 is separating tank, and 7 is rectifier, 8 is drop multiplication filler separation assembly, 9 is specific panel group formula phase separator assembly, 10 oil phase outlet plenums, and 11 is cyclone pipe, 12 is feed cavity, and 13 is oily(waste)water outlet plenum.
Embodiment
Following specific embodiment is intended to further illustrate the utility model device by reference to the accompanying drawings, instead of the scope of restriction the utility model claim protection.
The process of composition graphs 1 ~ 3 pair of the utility model device process cyclo-hexane oxidation waste alkali.
Cyclohexane oxide solution enters the first and second gravity separators and carries out gravity settling, and the residence time of each separator must not be less than 10 minutes, containing a small amount of pimelinketone, hexalin and a large amount of hexanaphthene composition organic phase and buck mutually major part be separated completely; Aqueous phase after gravity settling separation introduces vapo(u)rization system by pipeline, the organic phase obtained after separation enters drop multiplication separator, organic phase is introduced into original fluid container, enter again in separating tank, cooperatively interacted by drop multiplication filler separation assembly and specific panel group formula phase separator assembly and carry out drop multiplication and is separated, the time that liquid stops in drop doubles separator must not be less than 10 minutes; Aqueous phase after multiplication is separated introduces vapo(u)rization system, be separated the feed cavity that the organic phase obtained is introduced into cyclone separator, after being separated by cyclone pipe again, the oil phase of lightweight enters oil phase outlet plenum, the oil-water mixture of total mass enters oily(waste)water outlet plenum, and cyclone separator inlet outlet pressure differential is 0.1 ~ 0.25MPa; Enter coalescing separator again from cyclone separator oil phase outlet plenum organic phase out and carry out coarse separation, remove sodium ion in cyclohexane oxide solution.Cyclone separator oily(waste)water outlet plenum feed liquid out enters vapo(u)rization system.Organic phase after coalescing separator process finally enters alkane Tower System.
Embodiment 1
Certain produces 8.0 ten thousand tons of pimelinketone devices per year, and air flow is 13500 ~ 14500Nm 3/ h, the basicity of decomposition is 0.9 ~ 1.1mol/kg, and the inventory entering decomposition and separation system is 260 ~ 270t/h, and salkali waste separation circuit washing amount is 2.0m 3/ h, does not adopt the present invention, and the sodium ions content entered after separation in alkane distillation tower material is 5 ~ 8ppm, and the salkali waste amount delivering to salkali waste evaporization process is 12 ~ 13m 3/ h, the plant running cycle is 8 ~ 9 months.
Embodiment 2
Certain produces 8.0 ten thousand tons of pimelinketone devices per year, and air flow is 13500 ~ 14500Nm 3/ h, the basicity of decomposition is 0.9 ~ 1.1mol/kg, and the inventory entering decomposition and separation system is 260 ~ 270t/h, and adopt the present invention, the sodium ions content entered after separation in alkane distillation tower material is 6 ~ 8ppm, and the salkali waste amount delivering to salkali waste evaporization process is 10 ~ 11m 3/ h, the plant running cycle is 11 ~ 12 months.
Embodiment 3
Certain produces 8.0 ten thousand tons of pimelinketone devices per year, and air flow is 13500 ~ 14500Nm 3/ h, the basicity of decomposition is 0.9 ~ 1.1mol/kg, and the inventory entering decomposition and separation system is 260 ~ 270t/h, and salkali waste separation circuit washing amount is 0.5m 3/ h, adopt the present invention, the sodium ions content entered after separation in alkane distillation tower material is 3 ~ 7ppm, and the salkali waste amount delivering to salkali waste evaporization process is 10.5 ~ 11.5m 3/ h, the plant running cycle is more than 12 months.

Claims (5)

1. a cyclo-hexane oxidation waste alkali tripping device, it is characterized in that, be composed in series successively by pipeline by gravity separator (1), drop multiplication separator (2), cyclone separator (3) and coalescing separator (4).
2. cyclo-hexane oxidation waste alkali tripping device according to claim 1, is characterized in that, described drop multiplication separator (2) comprises original fluid container (5) and separating tank (6); Rectifier (7), drop multiplication filler separation assembly (8) and specific panel group formula phase separator assembly (9) is provided with in described separating tank.
3. cyclo-hexane oxidation waste alkali tripping device according to claim 2, it is characterized in that, original fluid container (5), rectifier (7), drop multiplication filler separation assembly (8) and specific panel group formula phase separator assembly (9) set gradually from the raw material upstream end of drop multiplication separator (2) to parting liquid output terminal.
4. cyclo-hexane oxidation waste alkali tripping device according to claim 1, is characterized in that, described gravity separator (1) adopts more than single-stage or two-stage to connect.
5. cyclo-hexane oxidation waste alkali tripping device according to claim 1, is characterized in that, described coalescing separator (4) adopts more than single-stage or two-stage to connect.
CN201420681600.4U 2014-11-12 2014-11-12 A kind of cyclo-hexane oxidation waste alkali tripping device Active CN204281488U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111875529A (en) * 2020-07-14 2020-11-03 中国石油化工股份有限公司 System and method for removing trace waste by CHPPO device
CN111892522A (en) * 2020-07-14 2020-11-06 中国石油化工股份有限公司 System and method for purifying oxidizing liquid of CHPPO device
CN113173839A (en) * 2021-04-28 2021-07-27 华东理工大学 Method and device for using discharged waste alkali liquor for micro-extraction of cyclohexane oxidation liquid

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111875529A (en) * 2020-07-14 2020-11-03 中国石油化工股份有限公司 System and method for removing trace waste by CHPPO device
CN111892522A (en) * 2020-07-14 2020-11-06 中国石油化工股份有限公司 System and method for purifying oxidizing liquid of CHPPO device
CN113173839A (en) * 2021-04-28 2021-07-27 华东理工大学 Method and device for using discharged waste alkali liquor for micro-extraction of cyclohexane oxidation liquid

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