CN109796334A - The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid - Google Patents
The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid Download PDFInfo
- Publication number
- CN109796334A CN109796334A CN201910134779.9A CN201910134779A CN109796334A CN 109796334 A CN109796334 A CN 109796334A CN 201910134779 A CN201910134779 A CN 201910134779A CN 109796334 A CN109796334 A CN 109796334A
- Authority
- CN
- China
- Prior art keywords
- kettle
- neopentyl glycol
- ester
- senko
- season
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000007788 liquid Substances 0.000 title claims abstract description 79
- 150000002148 esters Chemical class 0.000 title claims abstract description 52
- 239000002699 waste material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims description 62
- 230000008025 crystallization Effects 0.000 claims description 62
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 claims description 43
- 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 16
- 239000007791 liquid phase Substances 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 238000009434 installation Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 10
- 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
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 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
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 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
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000007599 discharging Methods 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001447 ferric ion Inorganic materials 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 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
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin 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
- 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 technique that the present invention provides intermittent to recycle season senko ester from 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.
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 it is a kind of it is intermittent from neopentyl glycol waste liquid recycle season senko ester technique.
Background technique
Hydroxypivalyl hydroxypivalate also known as season senko ester, 1115 esters can be used for preparing synthetic resin, unsaturation
Polyester, lubricating oil, car paint etc., because its two side stage of ester group has carbon atom, facile hydrolysis, not oxidizable, Gu synthesized by it
The features such as resin has stability good, pressure-resistant, wearability is strong, play an important role in high-end market field.In industrial production,
Hydrogenation method is prepared in the production process of neopentyl glycol, and the waste liquid generated when purifying neopentyl glycol product contains 40% season senko ester.
Every kilogram of senko ester of the season of content 97.5% reaches 140 yuan or more, therefore the utility in Recycling of waste liquid is to environment, economical
It is all significant.Season senko ester therein is generally recycled in production process by the way of rectifying.And the method is to new
Before pentanediol waste liquid carries out rectifying, ferric ion therein is not removed, causes product coloration not up to standard；Ferric ion
Oxidisability will cause product and be oxidized, and reduce product purity.Meanwhile Ji Xianke ester can decompose higher than 176 DEG C, using essence
It evaporates larger to temperature requirement harshness, energy consumption when tower separation season senko ester.
Summary of the invention
The technique of season senko ester is recycled in view of the above-mentioned problems, the present invention provides intermittent from 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 of product, improves the chromaticity index of product.In distillation process, carried out with lower temperature (being no more than 160 DEG C)
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 will not
It decomposes and generates new impurity, greatly reduce neopentyl glycol and season senko ester purifies difficulty.
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 season senko ester
Crystallization kettle；
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 intermittent technique that season senko ester is recycled from 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, 26 are 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, open feedstock valve, the raw materials of 6 tons of yellow by raw material pump with
Crystallization kettle is added in 200kg/min rate；
(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；
(5) 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+three
The sediment of valence iron ion；
(6) crystallization kettle bottom valve and collecting tank valve are opened, lower layer's water phase is made to remove collecting tank, is focused on, upper phase stays in kettle
It is interior；
(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. it is intermittent from neopentyl glycol waste liquid recycle season senko ester technique, specifically include that neopentyl glycol waste liquid raw material storage tank,
Recycle butyl butyrate storage tank, crystallization kettle, neopentyl glycol concentration kettle, neopentyl glycol purification kettle, neopentyl glycol crystallization kettle, Ji Xianke ester
Crystallization kettle, elevated tank with caustic soda liquid, butyl butyrate head tank, solid waste collecting tank, collecting tank, valve, collecting tank valve, crystallization kettle bottom
Valve, feedstock valve, recycle control valve, dried sodium sulfate dispensing port, is cycling in and out water installations, steam disengaging at collecting tank valve
Device, solid-liquid separator, gas-liquid separator, condenser, vacuum system, neopentyl glycol packaging system, agitating device, pump；Its mistake
Journey mainly includes decoloration dedoping step, material concentration process, neopentyl glycol purification process, Ji Xianke ester purification process；
The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid according to claim 1, 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. 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 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.
2. the intermittent technique for recycling season senko ester from neopentyl glycol waste liquid according to claim 1, feature exist
In:
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 intermittent technique for recycling season senko ester from neopentyl glycol waste liquid according to claim 1, feature exist
In:
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 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.
4. the intermittent technique for recycling season senko ester from neopentyl glycol waste liquid according to claim 1, feature exist
In season senko ester purification process technique it 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910134779.9A CN109796334A (en) | 2019-02-24 | 2019-02-24 | The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910134779.9A CN109796334A (en) | 2019-02-24 | 2019-02-24 | The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109796334A true CN109796334A (en) | 2019-05-24 |
Family
ID=66561253
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910134779.9A Withdrawn CN109796334A (en) | 2019-02-24 | 2019-02-24 | The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109796334A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0410167A1 (en) * | 1989-07-10 | 1991-01-30 | BASF Corporation | Method of producing 2,2,-dimethyl-3-hydroxypropyl-2,2-dimethyl-3-hydroxypropionate |
| WO1992007815A1 (en) * | 1990-10-29 | 1992-05-14 | Eastman Kodak Company | Process for the purification of hydroxypivalyl hydroxypivalate |
| DE10317545A1 (en) * | 2003-04-16 | 2004-11-04 | Basf Ag | Production of neopentyl glycol hydroxypivalate and neopentyl glycol comprises reacting isobutyraldehyde with formaldehyde and hydrogenating part of the product and disproportionating the rest |
| CN106966868A (en) * | 2017-04-06 | 2017-07-21 | 乐陵力维化学品有限责任公司 | A kind of production technology of neopentyl glycol raffinate recycling |
| 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 |
-
2019
- 2019-02-24 CN CN201910134779.9A patent/CN109796334A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0410167A1 (en) * | 1989-07-10 | 1991-01-30 | BASF Corporation | Method of producing 2,2,-dimethyl-3-hydroxypropyl-2,2-dimethyl-3-hydroxypropionate |
| WO1992007815A1 (en) * | 1990-10-29 | 1992-05-14 | Eastman Kodak Company | Process for the purification of hydroxypivalyl hydroxypivalate |
| DE10317545A1 (en) * | 2003-04-16 | 2004-11-04 | Basf Ag | Production of neopentyl glycol hydroxypivalate and neopentyl glycol comprises reacting isobutyraldehyde with formaldehyde and hydrogenating part of the product and disproportionating the rest |
| 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 |
| CN106966868A (en) * | 2017-04-06 | 2017-07-21 | 乐陵力维化学品有限责任公司 | A kind of production technology of neopentyl glycol raffinate recycling |
Non-Patent Citations (1)
| Title |
|---|
| 魏文德, 陕西科学技术出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116178105B (en) * | 2022-12-08 | 2024-05-14 | 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101654305B (en) | Process for changing phenolic nitrate effluent into useful material by extracting, evaporating, crystallizing and coupling | |
| CN101624400B (en) | Production method of triethyl phosphite | |
| CN102464573A (en) | Method for preparing high-purity resorcinol by melt crystallization | |
| CN105503530B (en) | Multiple-effect thermal coupling rectification production device and process prepared by alkaline process sodium methoxide | |
| CN208151005U (en) | A kind of epoxy resin high-salt wastewater concentration purification system | |
| CN106430228A (en) | Molecular sieve crystallization mother liquor treatment method | |
| CN102515112B (en) | Method for preparing sodium sulfide from hydrogen sulfide waste gas produced in production of viscose fibre | |
| CN114195102A (en) | Method and device for refining sulfur from desulfurized sulfur paste | |
| CN101182281A (en) | A method for refining biodiesel by-product glycerin | |
| CN109796334A (en) | The intermittent technique that season senko ester is recycled from neopentyl glycol waste liquid | |
| CN109400446A (en) | A kind of preparation method and equipment of p-cresol | |
| CN108821238A (en) | Blow out absorption process hydrobromic acid production method | |
| CN100503623C (en) | Process for preparing high-purity butoxy ethyl phosphate | |
| CN102827202B (en) | Technology for preparing diethyl phosphite by by-product of triethyl phosphite | |
| CN109761756A (en) | Process for extracting neopentyl glycol and quaternary ester from neopentyl glycol waste liquid | |
| CN106731582A (en) | A kind of method of integrated treatment sulfide hydrogen acid waste gas and solid waste carnallite | |
| CN207362101U (en) | A kind of crude naphthalene fine-processing production line | |
| CN109651088A (en) | The method for extracting neopentyl glycol in neopentyl glycol purifying waste liquid | |
| CN107722053A (en) | A kind of rectificating method of dimethylphosphite | |
| CN205616574U (en) | Use coking desulfurization waste liquid to carry device of salt extraction filter residue as raw materials purification sodium hyposulfite | |
| CN209193736U (en) | A kind for the treatment of process device of high-salt wastewater | |
| CN207405109U (en) | A kind of water-reducing agent production system | |
| CN109796308A (en) | A kind of intermittent technique that neopentyl glycol is recycled from neopentyl glycol waste liquid | |
| CN215886949U (en) | Ultrawhite stearic acid production device with low iodine value | |
| CN206970384U (en) | A kind of Zero discharging system of desulfurization wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190524 |
|
| WW01 | Invention patent application withdrawn after publication |