CN109651088A - The method for extracting neopentyl glycol in neopentyl glycol purifying waste liquid - Google Patents
The method for extracting neopentyl glycol in neopentyl glycol purifying waste liquid Download PDFInfo
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- CN109651088A CN109651088A CN201910134148.7A CN201910134148A CN109651088A CN 109651088 A CN109651088 A CN 109651088A CN 201910134148 A CN201910134148 A CN 201910134148A CN 109651088 A CN109651088 A CN 109651088A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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Abstract
Regarding to the issue above, the present invention provides the methods for extracting neopentyl glycol in neopentyl glycol purifying waste liquid to remove the ferric ion in waste liquid by way of lye is added under mild conditions before distilling to waste liquid, the purity for increasing product improves the chromaticity index of product.By the way that butyl butyrate is added, 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 purifying waste liquid in neopentyl glycol method.
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 better than by the resin property of Material synthesis of neopentyl glycol using ethylene glycol preparation
Resin, domestic neopentyl glycol manufacturing enterprise only have 11, and in the case where price is continuous high, still long-term supply falls short of demand, big portion
Divide and relies on import.Neopentyl glycol production method has discrimination method and comprehensive hydrogenation method at present, prepares the life of neopentyl glycol in hydrogenation method
During production, the waste liquid of generation contains 50% neopentyl glycol.The price of every kilogram of 99% neopentyl glycol is at 10 yuan or more, and to skin
Skin is irritant, therefore the utility recycled in this part waste liquid is all significant to environment, economy.In industrial production
Neopentyl glycol therein is recycled by way of rectifying.In traditional rectification process, before carrying out rectifying to neopentyl glycol waste liquid,
Ferric ion therein is not removed, and the oxidisability of ferric ion will cause product and be oxidized, and reduce product purity, also can shadow
Ring product coloration;In distillation process, neopentyl glycol can be crystallized in the case where being lower than 130 DEG C, block rectifying column, pipeline, because
This needs to heat pipeline, consumes big energy.
Summary of the invention
In view of the above-mentioned problems, the present invention provides the methods for extracting neopentyl glycol in neopentyl glycol purifying waste liquid, to useless
Before liquid is distilled, the ferric ion in waste liquid is removed by way of lye is added under mild conditions, increases production
The purity of product improves the chromaticity index of product.By the way that butyl butyrate is added, using entrained by the neopentyl glycol crude product distilled out
Heat so that butyl butyrate is gasified, be mixed into neopentyl glycol in T-shape interface and neopentyl glycol crude product meteorology after condensing
Butyl butyrate solution, solve the problems, such as neopentyl glycol lower than 130 DEG C of Crystallization Plugging pipelines, comparison is prevented with steam tracing
The method of crystallization eliminates the heating process to pipeline, can at least save 0.7t steam per hour, reduces production cost, increases
Economic benefit.And after the completion of the distillation of neopentyl glycol crude product, the butyl butyrate recycled is as recrystallization solvent, by straight
It connects and gradually cools down, slowly crystallization is precipitated, and the method being separated by filtration can directly obtain standard compliant neopentyl glycol product.It is 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 collecting tank valve is opened, lower layer's water phase is made to be delivered to collecting tank, upper liquid
Mutually stay in kettle;75kg desiccant sodium sulphate is added, stirs 30min, stops stirring, closing is cycling in and out water installations, stands
20min opens crystallization kettle bottom valve, valve and collecting tank valve, so that material in kettle is removed solid-liquid separator, solid material goes solid waste to receive
Collect slot, colourless liquid phase is delivered to neopentyl glycol concentration kettle by pump;
2. being added to neopentyl glycol concentration kettle from solid-liquid separator liquid phase, agitating device is opened;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 collecting tank;
During neopentyl glycol crystallizes near 10 DEG C of temperature in the kettle, there is solid precipitation, solidliquid mixture is transferred to solid-liquid separator, into
Row is separated by solid-liquid separation, and solid neopentyl glycol is delivered to neopentyl glycol packaging system, and liquid butyl butyrate is delivered to recycling butyl butyrate
Storage tank.
Detailed description of the invention
Fig. 1 is the method for extracting neopentyl glycol in neopentyl glycol purifying 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
It is feedstock valve for collecting tank, 21,22 be crystallization kettle bottom valve, 23 be recycle control valve, 24 is neopentyl glycol packaging system, 25
For collecting tank valve.
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 not be less than 30min, remain 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 25-30min, 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 collecting tank;
(15) during neopentyl glycol crystallizes near 10 DEG C of temperature in the kettle, there is solid precipitation, solidliquid mixture is transferred to solid-liquid
Separator is separated by solid-liquid separation, and solid neopentyl glycol is delivered to neopentyl glycol packaging system, and liquid butyl butyrate is delivered to recycling
Butyl butyrate storage tank.
Claims (2)
1. the method for extracting neopentyl glycol in neopentyl glycol purifying waste liquid, specifically includes that neopentyl glycol waste liquid raw material storage tank, recycling
Butyl butyrate storage tank, crystallization kettle, neopentyl glycol concentration kettle, neopentyl glycol purification kettle, neopentyl glycol 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, feedstock valve, reflux control
Valve processed, is cycling in and out water installations, steam in-out apparatus, solid-liquid separator, gas-liquid separator, condensation at dried sodium sulfate dispensing port
Device, vacuum system, neopentyl glycol packaging system, agitating device, pump;Its process mainly includes decoloration dedoping step, material concentration
Process, neopentyl glycol purification process;
The method according to claim 1 for extracting neopentyl glycol in neopentyl glycol purifying waste liquid, it is characterised in that:
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. 25-30min is stood, crystallization kettle bottom valve and collecting tank valve is opened, lower layer's water phase is made to be delivered to collecting tank, upper phase
It 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, valve and collecting tank valve are opened, so that material in kettle is removed solid-liquid separator, solid material goes solid waste collecting tank, nothing
Color liquid phase is delivered to neopentyl glycol concentration kettle by pump;
G. it is added to neopentyl glycol concentration kettle from solid-liquid separator liquid phase, opens agitating device;
H. steam in-out apparatus in neopentyl glycol concentration kettle is opened, makes the vapor (steam) temperature into neopentyl glycol concentration kettle 130
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;
I. 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.
2. the method according to claim 1 for extracting neopentyl glycol in neopentyl glycol purifying waste liquid, it is characterised in that:
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, 160-170 DEG C of the vapor (steam) temperature of neopentyl glycol purification kettle is opened
Vacuum system on gas-liquid separator, closing volume control valve are opened and are managed between neopentyl glycol purification kettle and neopentyl glycol crystallization kettle
All valves on line, system pressure 20kpa;Liquidus temperature rises to 160 DEG C (pressure 20kpa) in neopentyl glycol purification kettle kettle, newly
Gas phase enters neopentyl glycol crystallization kettle in pentanediol purification kettle, and neopentyl glycol crystallizes 85 DEG C of temperature in the kettle, neopentyl glycol crystallization kettle
Gas phase is ethyl butyrate in kettle, 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.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112142565A (en) * | 2020-09-18 | 2020-12-29 | 万华化学集团股份有限公司 | Neopentyl glycol refining and ester removing method and device system with low energy consumption |
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EP0410167A1 (en) * | 1989-07-10 | 1991-01-30 | BASF Corporation | Method of producing 2,2,-dimethyl-3-hydroxypropyl-2,2-dimethyl-3-hydroxypropionate |
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CN206799478U (en) * | 2017-04-04 | 2017-12-26 | 乐陵力维化学品有限责任公司 | The device of season SAST's fat is reclaimed in a kind of raffinate from neopentyl glycol |
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CN112142565B (en) * | 2020-09-18 | 2022-08-05 | 万华化学集团股份有限公司 | Neopentyl glycol refining and ester removing method and device system with low energy consumption |
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