CN109761756A - Process for extracting neopentyl glycol and quaternary ester from neopentyl glycol waste liquid - Google Patents
Process for extracting neopentyl glycol and quaternary ester from neopentyl glycol waste liquid Download PDFInfo
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- CN109761756A CN109761756A CN201910133408.9A CN201910133408A CN109761756A CN 109761756 A CN109761756 A CN 109761756A CN 201910133408 A CN201910133408 A CN 201910133408A CN 109761756 A CN109761756 A CN 109761756A
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- neopentyl glycol
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- liquid
- senko
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000007788 liquid Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002699 waste material Substances 0.000 title claims abstract description 24
- 125000004185 ester group Chemical group 0.000 title 1
- 238000002425 crystallisation Methods 0.000 claims abstract description 68
- 230000008025 crystallization Effects 0.000 claims abstract description 68
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 150000002148 esters Chemical class 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims description 35
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical class CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 238000003860 storage Methods 0.000 claims description 19
- 238000004064 recycling Methods 0.000 claims description 15
- 239000007791 liquid phase Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 239000012071 phase Substances 0.000 claims description 12
- 238000009434 installation Methods 0.000 claims description 11
- 230000001351 cycling effect Effects 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 239000002910 solid waste Substances 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000002274 desiccant Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 239000011343 solid material Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- 238000007599 discharging Methods 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 9
- 239000012043 crude product Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 5
- 229910001447 ferric ion Inorganic materials 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- RKLJSBNBBHBEOT-UHFFFAOYSA-N (3-hydroxy-2,2-dimethylpropanoyl) 3-hydroxy-2,2-dimethylpropanoate Chemical compound OCC(C)(C)C(=O)OC(=O)C(C)(C)CO RKLJSBNBBHBEOT-UHFFFAOYSA-N 0.000 description 1
- -1 Fe3+ ion Chemical class 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 238000005059 solid analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides the techniques for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid, before being distilled to waste liquid, the ferric ion in waste liquid is removed by way of lye is added under mild conditions, the purity of product is increased, improves the chromaticity index of product.In distillation process, rectifying is carried out with lower temperature (being no more than 160 DEG C), prevents season senko ester from being thermally decomposed, to make the output increased of season senko ester 30% or more, and season senko ester, which will not decompose, generates new impurity, greatly reduces neopentyl glycol and season senko ester purifies difficulty.And further through addition butyl butyrate, butyl butyrate is set to gasify using heat entrained by the neopentyl glycol crude product distilled out, the butyl butyrate solution of neopentyl glycol is mixed into T-shape interface and neopentyl glycol crude product meteorology after condensing, neopentyl glycol is solved the problems, such as lower than 130 DEG C of Crystallization Plugging pipelines, comparison prevents the method for crystallization with steam tracing, eliminates the heating process to pipeline, can at least save 0.7t steam per hour, production cost is reduced, economic benefit is increased.And after the completion of the distillation of neopentyl glycol crude product, the butyl butyrate recycled is as recrystallization solvent, and by directly gradually cooling down, slowly crystallization is precipitated, and the method being separated by filtration can directly obtain standard compliant neopentyl glycol product.Whole energy consumption is only 1/2 or so of the technique of rectifying column rectifying.
Description
Technical field
The invention belongs to technical field of petrochemical industry, are related to the by-product neopentyl glycol raffinate of hydrogenation method production neopentyl glycol
Technical application, specially extraction neopentyl glycol waste liquid in neopentyl glycol and season senko ester technique.
Background technique
Neopentyl glycol, abbreviation NPG is white crystalline solid mainly for the production of unsaturated-resin, oil-free alkyd resin, poly-
The plasticizer of polyurethane foam plastics and elastomer, surfactant, it may also be used for synthetic insulating material, printing ink, polymerization inhibitor,
Aeroengine oil oil dope etc. is synthesized, is a kind of important industrial chemicals, domestic neopentyl glycol is long-term, and supply falls short of demand, relies on
Import.It is poly- to can be used for preparing synthetic resin, unsaturation for Hydroxypivalyl hydroxypivalate also known as season senko ester, 1115 esters
The features such as ester, lubricating oil, car paint etc. have stability good by the resin that it is synthesized, pressure-resistant, wearability is strong.Current new penta
Glycol production method has discrimination method and comprehensive hydrogenation method, in the production process that hydrogenation method prepares neopentyl glycol, the waste liquid of generation
Contain 50% neopentyl glycol and 40% season senko ester, it is seen that wherein most is working substance.Every kilogram of 99% neopentyl glycol
Price is at 10 yuan or more, and every kilogram of senko ester of the season of content 97.5% even more reaches 140 yuan or more, therefore in Recycling of waste liquid
For utility to environment, economy is all significant.Recycled by way of rectifying in industrial production neopentyl glycol therein and
Ji Xianke ester.In traditional rectification process, before carrying out rectifying to neopentyl glycol waste liquid, ferric ion therein is not removed,
It is not up to standard to will cause product coloration；The oxidisability of ferric ion will cause product and be oxidized, and reduce product purity.Meanwhile season
Senko ester can decompose higher than 176 DEG C, harsh to temperature requirement when separating neopentyl glycol and season senko ester using rectifying column,
Energy consumption is larger, and in distillation process, and neopentyl glycol can be crystallized in the case where being lower than 130 DEG C, blocks rectifying column, pipeline,
Therefore it needs to heat pipeline, consumes big energy.
Summary of the invention
In view of the above-mentioned problems, the present invention provides the technique for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid,
Before distilling to waste liquid, the ferric ion in waste liquid is removed by way of lye is added under mild conditions, is increased
The purity for having added product improves the chromaticity index of product.In distillation process, with lower temperature (be no more than 160 DEG C) into
Row rectifying prevents season senko ester from being thermally decomposed, to make the output increased of season senko ester 30% or more, and season senko ester is not
It can decompose and generate new impurity, greatly reduce neopentyl glycol and season senko ester purifies difficulty.And further through be added butyl butyrate,
Butyl butyrate is set to gasify using heat entrained by the neopentyl glycol crude product distilled out, in T-shape interface and newly after condensing
Pentanediol crude product meteorology is mixed into the butyl butyrate solution of neopentyl glycol, and it is stifled in lower than 130 DEG C crystallizations to solve neopentyl glycol
The problem of filling in pipeline, comparison prevent the method for crystallization with steam tracing, eliminate the heating process to pipeline, at least may be used per hour
0.7t steam is saved, production cost is reduced, increases economic benefit.And it after the completion of the distillation of neopentyl glycol crude product, recycles
Butyl butyrate as recrystallization solvent, by directly gradually cooling down, slowly crystallization be precipitated, the method being separated by filtration can be direct
Obtain standard compliant neopentyl glycol product.Whole energy consumption is only 1/2 or so of the technique of rectifying column rectifying.
Present invention process process are as follows:
1, crystallization kettle is added by pump in the waste liquid in neopentyl glycol waste liquid raw material storage tank；Unlatching is cycling in and out water installations, beats simultaneously
Agitating device is opened, the raw material in crystallization kettle is kept for 20 DEG C or less；Be kept stirring under state, by 280kg concentration be 30% liquid alkaline with
Constant rate of speed 9kg/min instills crystallization kettle, and time for adding 30-40min is kept for 15-20 DEG C of temperature in the kettle；State is kept stirring,
Crystallization kettle is added with constant rate of speed 75kg/min in 3 tons of ethyl butyrates, time for adding 30-45min remains temperature in the kettle
15-20℃；20-30min is stood, crystallization kettle bottom valve and valve 1 is opened, so that lower layer's water phase is delivered to collecting tank, upper phase stays in
In kettle；75kg desiccant sodium sulphate is added, stirs 30min, stops stirring, closing is cycling in and out water installations, stands 20min, beats
Crystallization kettle bottom valve and valve 2 are opened, so that material in kettle is removed solid-liquid separator, solid material removes solid waste collecting tank, and colourless liquid phase passes through pump
It is delivered to neopentyl glycol concentration kettle；
2, it is added to neopentyl glycol concentration kettle from solid-liquid separator liquid phase, opens agitating device；Open neopentyl glycol concentration kettle
Upper steam in-out apparatus makes the vapor (steam) temperature into neopentyl glycol concentration kettle that neopentyl glycol concentration kettle heat up, beat at 125 DEG C
The vacuum system of recycling butyl butyrate storage tank is opened, opens neopentyl glycol concentration kettle to all pipelines between recycling butyl butyrate storage tank
Upper valve, system pressure 20kpa；When neopentyl glycol concentration temperature in the kettle reaches 85 DEG C, ethyl butyrate boiling, vapor condensation
Enter butyl butyrate storage tank afterwards, in butyl butyrate storage tank when 2.2-2.4 tons of butyl butyrates of recycling, stops steam disengaging system and add
Heat stops vacuum system work, is kept for 70-75 DEG C of temperature be transferred to neopentyl glycol purifying liquid phase in neopentyl glycol concentration kettle
Kettle；
3, neopentyl glycol purification kettle is added in the liquid phase from neopentyl glycol concentration kettle, while into neopentyl glycol crystallization kettle with rate
300kg ethyl butyrate is added in rate 75kg/min；Open steam in-out apparatus in neopentyl glycol purification kettle, neopentyl glycol purification kettle
165-170 DEG C of vapor (steam) temperature, open gas-liquid separator on vacuum system, closing volume control valve, open neopentyl glycol purifying
All valves on pipeline, system pressure 20kpa between kettle and neopentyl glycol crystallization kettle；Liquidus temperature in neopentyl glycol purification kettle kettle
It rises to 155-160 DEG C (pressure 20kpa), gas phase enters neopentyl glycol crystallization kettle, neopentyl glycol crystallization in neopentyl glycol purification kettle
80-90 DEG C of temperature in the kettle, gas phase is ethyl butyrate in neopentyl glycol crystallization kettle kettle, is gradually formed after condensing in gas-liquid separator
Stablize liquid level；After gas-liquid separator forms stable liquid level, recycle control valve is opened, purifies ethyl butyrate liquid and neopentyl glycol
Gas phase flows back to neopentyl glycol crystallization kettle simultaneously in kettle；In neopentyl glycol crystallization kettle when remaining 2.4 tons of materials, steam off disengaging dress
It sets, vacuum system, unlatching neopentyl glycol crystallization kettle, which is cycling in and out water installations, makes material in kettle cool down；Simultaneously by neopentyl glycol
1 ton of ethyl butyrate is added in purification kettle, makes temperature in the kettle to 70 DEG C, material in neopentyl glycol purification kettle is transferred to season senko ester
Crystallization kettle；During neopentyl glycol crystallizes near 10 DEG C of temperature in the kettle, there is solid precipitation, solidliquid mixture is transferred to solid-liquid point
It from device, is separated by solid-liquid separation, solid neopentyl glycol is delivered to neopentyl glycol packaging system, and liquid butyl butyrate is delivered to recycling fourth
Acid butyl ester storage tank；
4. the material from neopentyl glycol purification kettle is transferred in season senko ester crystallization kettle (65-70 DEG C of temperature), stirring dress is opened
It sets；Steam in-out apparatus is warming up to 85-90 DEG C to kettle in opening season senko ester crystallization kettle, opens simultaneously season senko ester crystallization kettle and follows
Ring water installations stablize 20min；Stop the heating of steam in-out apparatus, be kept stirring under working state of device, opens season senko ester knot
Water installations are cycling in and out on brilliant kettle, to being cooled to 0 DEG C in kettle；Solidliquid mixture is delivered to equipment for separating liquid from solid, solid season in kettle
Senko ester is delivered to season senko ester packaging system, and liquid ethyl butyrate liquid is collected to recycling butyl butyrate storage tank.
Detailed description of the invention
Fig. 1 is the technique for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid.
1 it is neopentyl glycol waste liquid head tank in figure, 2 be pump, 3 be valve, 4 be dried sodium sulfate dispensing port, 5 is liquid alkaline height
Position slot, 6 be butyl butyrate head tank, 7 be agitating device, 8 be cycling in and out water installations, 9 be steam in-out apparatus, 10 be crystallization
Kettle, 11 be solid-liquid separator, 12 be solid-liquid collecting tank, 13 be neopentyl glycol concentration kettle, 14 be condenser, 15 be vacuum system,
16 it is recycling butyl butyrate storage tank, 17 be gas-liquid separator, 18 be neopentyl glycol purification kettle, 19 is neopentyl glycol crystallization kettle, 20
For collecting tank, 21 be feedstock valve, 22 be crystallization kettle bottom valve, 23 be recycle control valve, 24 be season senko ester crystallization kettle, 25 be
Ji Xianke ester packaging system.
Specific embodiment
Below the technical scheme of the invention is illustrated by a specific example:
Embodiment 1:
(1) all valves of crystallization kettle crystallization kettle are closed, feedstock valve, raw material (neopentyl glycol 50%, season of 6 tons of yellow are opened
Senko ester 40%, water-soluble mixed alcohol impurity and Fe3+ ion 10%) it is pumped by raw material with 200kg/min rate addition crystallization kettle；
(2) recirculated water Inlet and outlet water is opened, stirring motor is opened simultaneously, starts to stir in kettle, recirculated water passes through collet for crystallization kettle
Interior raw material is cooled to 18 DEG C；
(3) be kept stirring under state, by elevated tank with caustic soda liquid by 280kg concentration be 30% liquid alkaline with constant rate of speed 9kg/min drop
Enter crystallization kettle, time for adding 30-40min remains 15-20 DEG C of temperature in the kettle；
(4) after liquid alkaline is added dropwise to complete, under the state that is kept stirring, by ethyl butyrate head tank by 5 tons of ethyl butyrates with constant
Crystallization kettle is added in rate, and time for adding 15min remains 15-20 DEG C of temperature in the kettle；
(6) after ethyl butyrate adds, static 20-30min, the interior layering of kettle, upper layer is that liquid phase is ethyl butyrate+neopentyl glycol+season
Senko ester+micro-moisture and impurity alcohol+micro water-soluble inorganic salt；Lower layer is water+water-solubility impurity alcohol+water-soluble inorganic salts+Fe3
The sediment of+ion；Crystallization kettle bottom valve is opened, lower layer's water phase is made to remove collecting tank, is focused on, upper phase stays in kettle；
(7) by solid feeding port, 75kg desiccant sodium sulphate is added, opens stirring 30min, stops stirring, close recirculated water
Inlet and outlet water, static 20min.Crystallization kettle bottom valve is opened, material in kettle is made to remove solid-liquid separator (solid-liquid separator), solid material
(hydrated sulfuric acid sodium and inorganic salts) go at solid waste collection to focus on, colourless liquid phase (+3 tons of neopentyl glycols+2.4 of 3 tons of ethyl butyrates
Ton season senko ester) concentration kettle gone by transfering material pump；
(8) 8.4 tons of mixed material liquid phases are added to neopentyl glycol concentration kettle through pipeline by solid-liquid separator, open stirring；
(9) condenser upper circulation water is opened into return water, opens steam inlet valve in concentration kettle, is controlled vapor (steam) temperature at 125 DEG C, is delayed
Slowly it heats up to neopentyl glycol concentration kettle, opens simultaneously recycling ethyl butyrate storage tank vacuum, open neopentyl glycol concentration kettle to recycling
Valve on all pipelines of ethyl butyrate storage tank, keeps system unimpeded, and keeping pressure in whole system is 20kpa；
(10) when neopentyl glycol concentration temperature in the kettle reaches 85 DEG C, ethyl butyrate boiling, gas phase is condensed by butyl butyrate condenser
To recycling ethyl butyrate storage tank storage, when 2.4 tons of butyl butyrates to be recycled, stops heating, stops vacuum, neopentyl glycol is concentrated
Liquid phase is transferred to neopentyl glycol purification kettle while hot in kettle；
(11) material is added to neopentyl glycol purification kettle from neopentyl glycol concentration kettle while hot, while passing through ethyl butyrate head tank
300kg ethyl butyrate is added to neopentyl glycol crystallization kettle neopentyl glycol crystallization kettle；
(12) butyl butyrate condenser recirculated water is opened, opens neopentyl glycol purification kettle steam (165-170 DEG C of vapor (steam) temperature), beats
Gas-liquid separator is opened, closing volume control valve is opened between other neopentyl glycol purification kettles and neopentyl glycol crystallization kettle on pipeline
All valves keep system internal pressure power in 20kpa.Liquidus temperature is gradually increased to 160 DEG C of (pressure in neopentyl glycol purification kettle kettle
20kpa), meteorological to remove neopentyl glycol crystallization kettle through No. 3 mouths of neopentyl glycol purification kettle, it is gradually stable that neopentyl glycol crystallizes temperature in the kettle
At 85 DEG C, meteorological in kettle is ethyl butyrate, in gas-liquid separator gas-liquid separator gradually shape after the condensation of butyl butyrate condenser
At stablizing liquid level；
(13) after gas-liquid separator forms stable liquid level.It is gradually opened recycle control valve, is ethyl butyrate liquid along pipeline and new
Meteorological in pentanediol purification kettle to flow back to neopentyl glycol crystallization kettle simultaneously, when beginning, pays attention to controlling recycle control valve aperture, guarantees gas
Level stability in liquid/gas separator；
(14) in neopentyl glycol purification kettle when remaining 2.4 tons of materials, stop steam, stop vacuum, open neopentyl glycol crystallization kettle,
Recirculated water is opened to cool down to material in kettle.1 ton of butyric acid is added into neopentyl glycol purification kettle by ethyl butyrate head tank simultaneously
Ethyl ester makes temperature in the kettle to 70 DEG C, and material in neopentyl glycol purification kettle is transferred to the crystallization of senko ester season, senko ester crystallization kettle season
Kettle；
(15) during neopentyl glycol crystallizes near 10 DEG C of temperature in the kettle, gradually there is solid precipitation, solidliquid mixture is transferred to
Solid-liquid separator is separated by solid-liquid separation, solid neopentyl glycol unlap process, and the collection of liquid butyl butyrate recycles；
(16) material is transferred to season senko ester crystallization kettle season senko ester crystallization kettle (temperature 70 C) in neopentyl glycol purification kettle, opens
Stirring；
(17) it opens steam in kettle and to kettle is warming up to 90 DEG C, open simultaneously butyl butyrate condenser recirculated water, stablize 20min；
(18) stop heating, be kept stirring under state, generation opens kettle upper circulation water, to being cooled to 0 DEG C in kettle, gradually there is solid analysis
Out；
(19) solidliquid mixture goes solid-liquid separator to be separated by solid-liquid separation in kettle, Ji Xianke ester solids package, ethyl butyrate liquid
It collects and recycles.
Claims (4)
1. extracting the technique of neopentyl glycol and season senko ester in neopentyl glycol waste liquid, specifically include that neopentyl glycol waste liquid raw material stores up
Tank, recycling butyl butyrate storage tank, crystallization kettle, neopentyl glycol concentration kettle, neopentyl glycol purification kettle, neopentyl glycol crystallization kettle, Ji Xian
Section's ester crystallization kettle, elevated tank with caustic soda liquid, butyl butyrate head tank, solid waste collecting tank, collecting tank, valve, crystallization kettle bottom valve, collecting tank
Valve, recycle control valve, dried sodium sulfate dispensing port, is cycling in and out water installations, steam in-out apparatus, solid-liquid at feedstock valve
Separator, gas-liquid separator, condenser, vacuum system, neopentyl glycol packaging system, agitating device, pump；Its process mainly includes
Decolourize dedoping step, material concentration process, neopentyl glycol purification process, Ji Xianke ester purification process；
The technique according to claim 1 for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid, feature exist
In:
A. crystallization kettle is added by pump in the waste liquid in neopentyl glycol waste liquid raw material storage tank；
B. it opens and is cycling in and out water installations, open simultaneously agitating device, the raw material in crystallization kettle is kept for 15-20 DEG C；
C. it is kept stirring under state, the liquid alkaline that 280kg concentration is 30% is instilled into crystallization kettle with constant rate of speed 9kg/min, when dropwise addition
Between 30min, keep 15-20 DEG C of temperature in the kettle；
D. it is kept stirring state, crystallization kettle is added with constant rate of speed in 3 tons of ethyl butyrates, time for adding 15min remains kettle
15-20 DEG C of interior temperature；
E. 20-30min is stood, crystallization kettle bottom valve, valve and collecting tank valve is opened, lower layer's water phase is made to be delivered to collecting tank, on
Layer liquid phase stays in kettle；
F. 75kg desiccant sodium sulphate is added, stirs 30min, stops stirring, closing is cycling in and out water installations, stands 20min, beats
Crystallization kettle bottom valve and valve 2 are opened, so that material in kettle is removed solid-liquid separator, solid material removes solid waste collecting tank, and colourless liquid phase passes through pump
It is delivered to neopentyl glycol concentration kettle.
2. the technique according to claim 1 for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid, feature
It is:
A. it is added to neopentyl glycol concentration kettle from solid-liquid separator liquid phase, opens agitating device；
B. steam in-out apparatus in neopentyl glycol concentration kettle is opened, makes the vapor (steam) temperature into neopentyl glycol concentration kettle 125
DEG C, neopentyl glycol concentration kettle is heated up, the vacuum system of recycling butyl butyrate storage tank is opened, neopentyl glycol concentration kettle is opened and extremely returns
Receive between butyl butyrate storage tank valve, system pressure 20kpa on all pipelines；
C. when neopentyl glycol concentration temperature in the kettle reaches 85 DEG C, ethyl butyrate boils, and butyl butyrate is entered after vapor condensation and is stored up
Tank in butyl butyrate storage tank when 2.4 tons of butyl butyrates of recycling, stops the heating of steam disengaging system, stops vacuum system work, will
Liquid phase is kept for 75 DEG C and is transferred to neopentyl glycol purification kettle in neopentyl glycol concentration kettle.
3. the technique according to claim 1 for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid, feature
It is:
A. liquid phase from neopentyl glycol concentration kettle is added neopentyl glycol purification kettle, while with rate 75kg/min to neopentyl glycol
300kg ethyl butyrate is added in crystallization kettle；
B. steam in-out apparatus in neopentyl glycol purification kettle is opened, 165-170 DEG C of the vapor (steam) temperature of neopentyl glycol purification kettle is inflated
Vacuum system on liquid/gas separator, closing volume control valve open pipeline between neopentyl glycol purification kettle and neopentyl glycol crystallization kettle
Upper all valves, system pressure 20kpa；Liquidus temperature rises to 160 DEG C (pressure 20kpa) in neopentyl glycol purification kettle kettle, and new penta
Gas phase enters neopentyl glycol crystallization kettle in glycol purification kettle, and neopentyl glycol crystallizes 85 DEG C of temperature in the kettle, neopentyl glycol crystallization kettle kettle
Interior gas phase is ethyl butyrate, gradually forms stable liquid level in gas-liquid separator after condensing；
C. after gas-liquid separator forms stable liquid level, recycle control valve is opened, ethyl butyrate liquid and neopentyl glycol purification kettle are made
Interior gas phase flows back to neopentyl glycol crystallization kettle simultaneously；
D. in neopentyl glycol crystallization kettle when remaining 2.4 tons of materials, steam off in-out apparatus, vacuum system open neopentyl glycol
Crystallization kettle, which is cycling in and out water installations, makes material in kettle cool down；Simultaneously by the way that 1 ton of ethyl butyrate is added into neopentyl glycol purification kettle,
Make temperature in the kettle to 70 DEG C, material in neopentyl glycol purification kettle is transferred to season senko ester crystallization kettle；
E. during neopentyl glycol crystallizes near 10 DEG C of temperature in the kettle, there is solid precipitation, solidliquid mixture is transferred to solid-liquid point
It from device, is separated by solid-liquid separation, solid neopentyl glycol is delivered to neopentyl glycol packaging system, and liquid butyl butyrate is delivered to recycling fourth
Acid butyl ester storage tank.
4. the technique according to claim 1 for extracting neopentyl glycol and season senko ester in neopentyl glycol waste liquid, feature
It is that season senko ester purification process technique is as follows:
A. the material from neopentyl glycol purification kettle is transferred in season senko ester crystallization kettle (temperature 70 C), opens agitating device；
B. it opens steam in-out apparatus in season senko ester crystallization kettle and to kettle is warming up to 90 DEG C, open simultaneously season senko ester crystallization kettle and follow
Ring water installations stablize 20min；
C. stop steam in-out apparatus heating, be kept stirring under working state of device, open season senko ester crystallization kettle on recycle into
Discharging device, to being cooled to 0 DEG C in kettle；
D. solidliquid mixture is delivered to equipment for separating liquid from solid in kettle, solid season senko ester be delivered to season senko ester packaging system, liquid
Body ethyl butyrate liquid is collected to recycling butyl butyrate storage tank.
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Cited By (1)
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| CN116178105A (en) * | 2022-12-08 | 2023-05-30 | 万华化学集团股份有限公司 | Method for improving neopentyl glycol yield by catalytic decomposition of quaternary congenital ester |
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| CN116178105A (en) * | 2022-12-08 | 2023-05-30 | 万华化学集团股份有限公司 | Method for improving neopentyl glycol yield by catalytic decomposition of quaternary congenital ester |
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