CN105837621B - A kind of after-treatment device and method of phosphate flame retardant - Google Patents
A kind of after-treatment device and method of phosphate flame retardant Download PDFInfo
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- CN105837621B CN105837621B CN201510021040.9A CN201510021040A CN105837621B CN 105837621 B CN105837621 B CN 105837621B CN 201510021040 A CN201510021040 A CN 201510021040A CN 105837621 B CN105837621 B CN 105837621B
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Abstract
The present invention provides a kind of after-treatment device of phosphate flame retardant and method, the after-treatment device of the phosphate flame retardant includes：Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and discharge port；The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharge port；The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port, are used for output phosphate flame retardant.Compared with prior art, the after-treatment device of phosphate flame retardant provided by the invention can improve the mass transfer effect of storeroom in last handling process, and product has higher yield after ensureing post-processing.The experimental results showed that being post-processed using device provided by the invention, obtained phosphate flame retardant yield is 94% or more.
Description
Technical field
The present invention relates to phosphate flame retardant production technical fields, are to be related to a kind of phosphate flame retardant more specifically
After-treatment device and method.
Background technology
Phosphate flame retardant is world's second largest fire retardant kind, and the global output value reaches 1,200,000,000 dollars or so.With other resistances
Combustion agent compare, phosphate flame retardant have flame retardant effect it is lasting, it is good with polymeric matrix compatible, it is water-fast, weather-proof, heat-resisting and
The features such as resistance to migration, has irreplaceable critical role in polymeric material fields such as polyurethane.Increasingly with environmental requirement
It improves, the application range of the halogen flames such as traditional bromine system is limited by different degrees of, and phosphate flame retardant belongs to ring
Border friendly fire retardant, following market prospects are very good.
Phosphate flame retardant production process is broadly divided into two processes of esterification and post-processing, as shown in FIG. 1, FIG. 1 is
The existing production technological process of phosphate flame retardant.Wherein, no matter postprocessing working procedures are in the side such as equipment investment or production cost
Face all accounts for very important status.Currently, in terms of the postprocessing working procedures of phosphate ester product, traditional method includes following
Step：Pickling, alkalinity, washing, dehydration and filtering, the mode of production of use are the intervals of pickling kettle, alkali cleaning kettle and washing kettle etc.
Operation.
But not only device capbility is small for traditional post-processing approach, but also unstable product quality, it is often more important that due to
Phosphate itself has hydrolyzable, and product is long with the times of contact such as acid, alkali and water in last handling process, can influence product
Yield.
Invention content
In view of this, the purpose of the present invention is to provide a kind of after-treatment device of phosphate flame retardant and method, use
Device and method provided by the invention are post-processed, the high income of obtained phosphate ester product.
The present invention provides a kind of after-treatment devices of phosphate flame retardant, including：
Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and discharging
Mouthful；
The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharging
Mouthful；
The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port,
For output phosphate flame retardant.
Preferably, further include：
Alkali storage device for preparing and storing lye；The feed inlet of the alkali storage device and the caustic wash tower
It is connected.
Preferably, the caustic wash tower feed inlet, lye import, water scrubber feed inlet and technique water inlet are respectively arranged with stream
Amount control device.
Preferably, further include：
Filter；The filter is connected with the discharge port of the thin film evaporator.
The present invention also provides a kind of post-processing approach of phosphate flame retardant, include the following steps：
A) phosphate crude product and lye are subjected to the first counter current contacting, obtain the phosphate after alkali cleaning；
B) phosphate after alkali cleaning is subjected to the second counter current contacting, the phosphate after being washed with water；
C) phosphate after washing is subjected to thin film evaporation, obtains phosphate flame retardant.
Preferably, the lye is one kind in aqueous sodium carbonate, sodium hydrate aqueous solution and potassium hydroxide aqueous solution
Or it is a variety of.
Preferably, a concentration of the 5%~15% of the lye.
Preferably, during the first counter current contacting described in step a), the flow of the lye and the phosphate crude product
Flow-rate ratio be (8~25)：100；The time of first counter current contacting is 7min~20min.
Preferably, during the second counter current contacting described in step b), the flow of the water and the phosphoric acid after the alkali cleaning
The flow-rate ratio of ester is (20~50)：100；The time of second counter current contacting is 8min~30min.
Preferably, the step c) further includes：
Phosphate after thin film evaporation is filtered.
The present invention provides a kind of after-treatment device of phosphate flame retardant and method, the rear place of the phosphate flame retardant
Managing device includes：Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and go out
Material mouth；The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharge port；
The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port, are used for output
Phosphate flame retardant.Compared with prior art, the after-treatment device of phosphate flame retardant provided by the invention is first by phosphate
Crude product is added to caustic wash tower with lye and carries out counter current contacting simultaneously, obtains the phosphate after alkali cleaning；Then by the phosphoric acid after alkali cleaning
Ester is added to water scrubber with water and carries out counter current contacting, the phosphate after being washed simultaneously；Finally the phosphate after washing is added
Enter to thin film evaporator and carry out thin film evaporation, obtains phosphate flame retardant.The post-processing of phosphate flame retardant provided by the invention
Device realizes the serialization of product post-processing, avoids traditional handicraft since product quality fluctuation caused by human factor is larger
The problem of, obtained product quality is stablized；Importantly, the after-treatment device of phosphate flame retardant provided by the invention can
The mass transfer effect of storeroom in last handling process is improved, product has higher yield after ensureing post-processing.The experimental results showed that
It is post-processed using device provided by the invention, obtained phosphate flame retardant yield is 94% or more.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the existing production technological process of phosphate flame retardant；
Fig. 2 is the structural schematic diagram of the after-treatment device of phosphate flame retardant provided in an embodiment of the present invention；
Fig. 3 is the structural schematic diagram of the after-treatment device for the phosphate flame retardant that the embodiment of the present invention 1 provides.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of after-treatment devices of phosphate flame retardant, including：
Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and discharging
Mouthful；
The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharging
Mouthful；
The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port,
For output phosphate flame retardant.
Referring to Fig. 2, Fig. 2 is the structural representation of the after-treatment device of phosphate flame retardant provided in an embodiment of the present invention
Figure, wherein 1 is caustic wash tower, and 2 be caustic wash tower feed inlet, and 3 be lye import, and 4 be caustic wash tower discharge port, and 5 be water scrubber, and 6 be water
Tower feed inlet is washed, 7 be technique water inlet, and 8 be water scrubber discharge port, and 9 be thin film evaporator, and 10 be thin film evaporator feed inlet,
11 be thin film evaporator discharge port, and 12 be alkali storage device, and 13~16 be volume control device, and 17 be filter.
In the present invention, the caustic wash tower (1) is used to carry out alkali cleaning, preferably sieve-plate tower or filler to phosphate crude product
Tower, more preferably sieve-plate tower；Caustic wash tower (1) used in the embodiment of the present invention 1 is vibrating sieve plate tower.In the present invention, described
Phosphate crude product is obtained not post-treated phosphate after esterification, the phosphate crude product without pickling, directly into
Enter caustic wash tower (1), since pickling processes are to the washing effect unobvious of phosphate crude product, device pair provided in an embodiment of the present invention
Pickler is simplified.
In the present invention, be provided with caustic wash tower feed inlet (2) at the top of the caustic wash tower (1), for by phosphate crude product into
Material to caustic wash tower (1) carries out alkali cleaning；Caustic wash tower (1) bottom is respectively arranged with lye import (3) and caustic wash tower discharge port
(4), wherein the lye import (3) makes lye to the phosphoric acid for prepared lye to be delivered in caustic wash tower (1)
Ester crude product carries out alkali cleaning；The caustic wash tower discharge port (4) continues subsequent processing for the phosphate after alkali cleaning to discharge.
In the present invention, it is provided with volume control device (13) on the caustic wash tower feed inlet (2), for entering alkali cleaning
The flow of the phosphate crude product of tower (1) is controlled；It is provided with volume control device (14) on the lye import (3), is used for
The flow of lye to entering caustic wash tower (1) controls.The present invention is not particularly limited the volume control device, such as may be used
Using delivery pump well known to those skilled in the art.
In a preferred embodiment of the invention, the lye import (3) is connected with alkali storage device (12)；The lye
Storage device (12) is for preparing and storing lye.
In the present invention, the phosphate crude product that the caustic wash tower (1) can prepare esterification is carried out continuously alkali cleaning, phosphorus
Acid esters crude product and lye carry out alkali cleaning by counter current contacting, that is, it is long with lye time of contact and occur to avoid phosphate crude product
Hydrolysis, and the mass transfer effect of phosphate crude product and lye is improved, while ensureing product yield to reach, when shortening alkali cleaning
Between and reduce waste water yield effect.
In the present invention, the water scrubber (5) is for washing the phosphate after alkali cleaning, preferably sieve-plate tower or fills out
Expect tower, more preferably sieve-plate tower；Water scrubber (5) used in the embodiment of the present invention 1 is vibrating sieve plate tower.
In the present invention, water scrubber feed inlet (6), the water scrubber feed inlet (6) are provided at the top of the water scrubber (5)
Being connected with the caustic wash tower discharge port (4), being washed for feeding the phosphate after alkali cleaning to water scrubber (5)；It is described
Water scrubber (5) bottom is respectively arranged with technique water inlet (7) and water scrubber discharge port (8), wherein the technique water inlet (7)
For water to be delivered in water scrubber (5), water is made to wash the phosphate after the alkali cleaning；The water scrubber discharge port
(8) it is used to discharge the phosphate after washing, continues subsequent processing.
In the present invention, it is provided with volume control device (15) on the water scrubber feed inlet (6), for being washed to entering
The flow of phosphate after the alkali cleaning of tower (5) is controlled；It is provided with volume control device on the technique water inlet (7)
(16), the flow for being used for the water to entering water scrubber (5) controls.The present invention does not have special limit to the volume control device
System, such as can be used delivery pump well known to those skilled in the art.
In the present invention, the water scrubber (5) can be carried out continuously washing to the phosphate after alkali cleaning, the phosphoric acid after alkali cleaning
Ester is washed with water by counter current contacting, that is, it is long with water time of contact and hydrolyze to avoid the phosphate after alkali cleaning,
The mass transfer effect for improving phosphate and water after alkali cleaning again while ensureing product yield to reach, shortens washing time
And reduce the effect of waste water yield.
In the present invention, the thin film evaporator (9) preferably rises film and steams for being distilled to the phosphate after washing
Send out device or falling film evaporator；Thin film evaporator (9) used in the embodiment of the present invention 1 is falling film evaporator.
In the present invention, thin film evaporator feed inlet (10) is provided at the top of the thin film evaporator (9), the film steams
Hair device feed inlet (10) is connected with water scrubber discharging (8), for feeding the phosphate after washing to thin film evaporator
(9) it is distilled；Thin film evaporator (9) bottom is provided with thin film evaporator discharge port (11), for being obtained after distilling
Phosphate flame retardant discharge.
In the present invention, the thin film evaporator (9) has the characteristics that heat exchange area is big, good effect of heat exchange, using film
Evaporation is carried out continuously distillation to the phosphate after washing, not only increases production efficiency, and reduce the energy in distillation process
Consumption, while being combined with above-mentioned caustic wash tower (1), water scrubber (5), the serialization of phosphate crude product post-processing is realized, is significantly improved
The production capacity of device.
In a preferred embodiment of the invention, the thin film evaporator discharge port (11) is connected with filter (17)；It is described
Filter (17) completes the post-processing of phosphate crude product for being filtered to the phosphate after thin film evaporation.
According to the after-treatment device for the phosphate flame retardant that the embodiments of the present invention provide, post-processing can be improved and obtained
Phosphate flame retardant yield.The course of work of the embodiment of the present invention is as follows：
First, phosphate crude product is controlled into flow through flow controller (13), then enters alkali cleaning through caustic wash tower feed inlet (2)
Tower (1), while the lye in alkali storage device (12) is controlled into flow through flow controller (14), then through lye import (3)
Into caustic wash tower (1), the phosphate crude product and lye counter current contacting carry out alkali cleaning, obtain the phosphate after alkali cleaning through alkali cleaning
Caustic wash tower (1) is discharged in tower discharge port (4)；
Secondly, flow will be controlled through flow controller (15) by the phosphate after the alkali cleaning of caustic wash tower discharge port (4) discharge,
Enter water scrubber (5) through water scrubber feed inlet (6) again, while water is controlled into flow through flow controller (16), then through process water
Import (7) enters water scrubber (5), the phosphate after the alkali cleaning and water counter current contacting, is washed, the phosphoric acid after being washed
Ester is through water scrubber discharge port (8) discharge water scrubber (5)；
Again, will by water scrubber discharge port (8) be discharged washing after phosphate through thin film evaporator feed inlet (10) into
Enter thin film evaporator (9) to be distilled, obtains phosphate flame retardant and thin film evaporator is discharged through thin film evaporator discharge port (11)
(9)；
Finally, obtained phosphate flame retardant is filtered, completes the post-processing of phosphate crude product.
The present invention also provides a kind of post-processing approach of phosphate flame retardant, include the following steps：
A) phosphate crude product and lye are subjected to the first counter current contacting, obtain the phosphate after alkali cleaning；
B) phosphate after alkali cleaning is subjected to the second counter current contacting, the phosphate after being washed with water；
C) phosphate after washing is subjected to thin film evaporation, obtains phosphate flame retardant.
In the present invention, phosphate crude product and lye are subjected to the first counter current contacting, obtain the phosphate after alkali cleaning.It is described
Phosphate crude product is mainly the not post-treated intermediate products obtained after esterification, and impurity includes unreacted raw material, urges
Agent and by-product.In the present invention, the phosphate crude product can be three (chloro isopropyl) phosphates, three (β-ethyl) phosphoric acid
Ester, trimethyl phosphate, triethyl phosphate, tricresyl phosphate second propyl phenyl ester, bisphenol-A-(diphenyl phosphoester) or resorcinol-are (double
Diphenyl phosphoester) crude product.The phosphate crude product directly carries out alkali cleaning without pickling, since pickling processes are to phosphate
The washing effect unobvious of crude product, method provided by the invention simplify pickling link.In the present invention, simplify pickling ring
On the one hand section directly avoids phosphate crude product and contacts and hydrolyze with acid solution, on the other hand cut down the yield of waste water.
In the present invention, the lye is preferably aqueous sodium carbonate, sodium hydrate aqueous solution and potassium hydroxide aqueous solution
In one or more, more preferably aqueous sodium carbonate.In the present invention, the concentration of the lye is preferably 5%~15%,
More preferably 10%.
In embodiments of the present invention, the first counter current contacting process carries out in caustic wash tower (1), the flow of the lye
Flow-rate ratio with the phosphate crude product is preferably (8~25)：100, more preferably 15：100；First counter current contacting when
Between preferably 7min~20min, more preferably 10min.The present invention by control concentration of lye and lye and phosphate crude product into
The flow of row counter current contacting eliminates the fuel factor that chemical reaction is brought, it is often more important that the generation for avoiding emulsion ensure that
The yield of phosphate flame retardant, while realizing the serialization of alkaline cleaning procedure.
After obtaining the phosphate after alkali cleaning, the phosphate after alkali cleaning is carried out the second counter current contacting by the present invention with water, is obtained
Phosphate after washing.Second counter current contacting process described in the embodiment of the present invention carries out in water scrubber (5), the flow of the water
Flow-rate ratio with the phosphate after the alkali cleaning is preferably (20~50)：100, more preferably 20：100；Second adverse current connects
The tactile time is preferably 8min~30min, more preferably 10min.The present invention is carried out by controlling water with the phosphate after alkali cleaning
The flow of counter current contacting in the phosphate after removing alkali cleaning while remaining alkali, reduces phosphoric acid ester hydrolysis and in water
In dissolving, avoid the generation of emulsion, play an important role in terms of the yield to ensureing phosphate flame retardant, while realizing water
Wash the serialization of journey.
After phosphate after being washed, the phosphate after washing is carried out thin film evaporation by the present invention, obtains phosphate resistance
Fire agent.Thin film evaporation process described in the embodiment of the present invention carries out in thin film evaporator (9), and the purpose of the thin film evaporation is pair
Phosphate after washing is distilled, and realizes the dehydration of the phosphate after washing.The time of the thin film evaporation is preferably 30min
~40min, more preferably 35min.The present invention enhances the heat transfer effect in distillation process by using thin film evaporation, to drop
Low energy consumption, improves production efficiency, while realizing the serialization of phosphate crude product post-processing.
After obtaining phosphate flame retardant, the present invention preferably further includes：
Phosphate after thin film evaporation is filtered.Filter process described in the embodiment of the present invention in filter (17) into
The method of row, the filtering is technological means well known to those skilled in the art, and it is not specifically limited to this by the present invention.
The present invention provides a kind of after-treatment device of phosphate flame retardant and method, the rear place of the phosphate flame retardant
Managing device includes：Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and go out
Material mouth；The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharge port；
The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port, are used for output
Phosphate flame retardant.Compared with prior art, the after-treatment device of phosphate flame retardant provided by the invention is first by phosphate
Crude product is added to caustic wash tower with lye and carries out counter current contacting simultaneously, obtains the phosphate after alkali cleaning；Then by the phosphoric acid after alkali cleaning
Ester is added to water scrubber with water and carries out counter current contacting, the phosphate after being washed simultaneously；Finally the phosphate after washing is added
Enter to thin film evaporator and carry out thin film evaporation, obtains phosphate flame retardant.The post-processing of phosphate flame retardant provided by the invention
Device realizes the serialization of product post-processing, easy to operate, greatly reduces labor operations intensity and improves operating environment,
Traditional handicraft is also avoided since product quality caused by human factor fluctuates larger problem, obtained product quality is stablized；
Importantly, the after-treatment device of phosphate flame retardant provided by the invention can improve the biography of storeroom in last handling process
Matter effect, product has higher yield after ensureing post-processing.The experimental results showed that after being carried out using device provided by the invention
Processing, obtained phosphate flame retardant yield is 94% or more.The present invention replaces Conventional espresso using thin-film evaporation proc simultaneously
Kettle technique, enhances heat transfer effect, and steam energy consumption reduces by 30% or more.
In addition, the after-treatment device of phosphate flame retardant provided by the invention is not influencing product yield and post-processing effect
On the basis of, it optimizes, is not necessarily to pickling, reduces equipment investment, simplify operation, can also reduce the generation of pickling waste waters,
Reduce cost.
In order to further illustrate the present invention, it is described in detail below by following embodiment.In the embodiment of the present invention 1
In, phosphate crude product used is three (chloro isopropyl) phosphate crude products, and product content is 78~88%, impurity and its content point
It is not：Propylene oxide 0.1%~5%, catalyst (titanium tetrachloride or alchlor or magnesium chloride etc.) 0.01%~2%, phosphoric acid
0.1%~3%, the other impurity such as aldehydes 5%~10%；In the embodiment of the present invention 2, phosphate crude product used is three (β-
Ethyl) phosphate crude product, product content is 80%~90%, and impurity and its content are respectively：Ethylene oxide 0.1%~5%, is urged
Agent (titanium tetrachloride or alchlor or magnesium chloride etc.) 0.01%~2%, phosphoric acid 0.1%~3%, other impurity such as aldehydes
5%~10%；In the embodiment of the present invention 3, phosphate crude product used is bisphenol-A-(diphenyl phosphoester) crude product, and product contains
Amount is 80%~90%, and impurity and its content are：Phenol 0.5%~5%, bisphenol-A 0.1%~2%, phosphoric acid 0.5%~2%,
Hydrogen chloride 0.1%~1%, other impurity 2%~10%.
Embodiment 1
The structural schematic diagram of the after-treatment device for the phosphate flame retardant that embodiment 1 provides is as shown in Figure 3.Wherein, 1 is alkali
Wash tower, 2 be caustic wash tower feed inlet, and 3 be lye import, and 4 be caustic wash tower discharge port, and 5 be water scrubber, and 6 be water scrubber feed inlet, 7
It is water scrubber discharge port for technique water inlet, 8,9 be thin film evaporator, and 10 be thin film evaporator feed inlet, and 11 be thin film evaporation
Device discharge port, 12 be alkali storage device, and 13~16 be delivery pump, and 17 be filter, and 18 export for alkali-wash waste water, and 19 be washing
Wastewater outlet, 20 be distillation wastewater outlet, and 21 be condenser, and 22 be steam inlet, and 23 be condensation-water drain.
The caustic wash tower (1) is vibrating sieve plate tower.It is respectively arranged with caustic wash tower feed inlet (2) at the top of the caustic wash tower (1)
(18) are exported with alkali-wash waste water, wherein the lye import (3) is connected with alkali storage device (12)；The caustic wash tower into
Delivery pump (13) is provided in material mouth (2)；The alkali-wash waste water outlet (18) is for being discharged the waste water after alkali cleaning.The caustic wash tower
(1) bottom is respectively arranged with lye import (3) and caustic wash tower discharge port (4), wherein is provided on the lye import (3) defeated
Send pump (14)；The caustic wash tower discharge port (4) is connected with the water scrubber (5).
The water scrubber (5) is vibrating sieve plate tower.It is respectively arranged with water scrubber feed inlet (6) at the top of the water scrubber (5)
(19) are exported with washing waste water, wherein the water scrubber feed inlet (6) is connected with the caustic wash tower discharge port (4)；The water
It washes on tower feed inlet (6) and is provided with delivery pump (15)；The washing waste water outlet (19) is used to that the waste water after washing to be discharged.It is described
Water scrubber (5) bottom is respectively arranged with technique water inlet (7) and water scrubber discharge port (8), wherein the technique water inlet (7)
On be provided with delivery pump (16)；The water scrubber discharge port (8) is connected with the thin film evaporator (9).
The thin film evaporator (9) is falling film evaporator.It is respectively arranged with thin film evaporation at the top of the thin film evaporator (9)
Device feed inlet (10) and distillation wastewater outlet (20), wherein the thin film evaporator feed inlet (10) discharges with the water scrubber
Mouth (8) is connected；The distillation wastewater outlet (20) is used to that the waste water after distillation to be discharged；The distillation wastewater outlet (20) with it is cold
Condenser (21) is connected, and the condenser (21) is used to condense distillation waste water.Thin film evaporator (9) the bottom setting
There is thin film evaporator discharge port (11).The thin film evaporator discharge port (11) is connected with filter (17).The film steams
Hair device (9) is passed through steam by steam inlet (22), carries out thin film evaporation, and obtained condensed water is arranged by condensation-water drain (23)
Go out.
It is post-processed in the after-treatment device for the phosphate flame retardant that above-described embodiment 1 provides, the phosphate resistance
Combustion agent the after-treatment device course of work be specially：
(1) it is 100kg/h through delivery pump (13) control flow by 500kg phosphates crude product, then through caustic wash tower feed inlet (2)
Into caustic wash tower (1), while by a concentration of 10% aqueous sodium carbonate in alkali storage device (12) through delivery pump (14)
Control flow is 15kg/h, then enters caustic wash tower (1) through lye import (3), and the phosphate crude product and aqueous sodium carbonate are inverse
Stream contact 10min, carries out alkali cleaning, obtains the phosphate after alkali cleaning through caustic wash tower discharge port (4) discharge caustic wash tower (1), alkali cleaning is useless
Water is through alkali-wash waste water outlet (18) discharge caustic wash tower (1)；
(2) it is through delivery pump (15) control flow by the phosphate after the alkali cleaning being discharged by caustic wash tower discharge port (4)
100kg/h, then enter water scrubber (5) through water scrubber feed inlet (6), while being 20kg/ through delivery pump (16) control flow by water
H, then enter water scrubber (5), the phosphate after the alkali cleaning and water counter current contacting 10min through technique water inlet (7), carry out water
It washes, through water scrubber discharge port (8) discharge water scrubber (5), washing waste water exports the phosphate after being washed through washing waste water
(19) discharge water scrubber (5)；
(3) will be entered through thin film evaporator feed inlet (10) by the phosphate after the washing of water scrubber discharge port (8) discharge
Thin film evaporator (9), thin film evaporator (9) are passed through steam by steam inlet (22), and obtained condensed water is gone out by condensed water
Mouth (23) discharge；Phosphate after washing carries out thin film evaporation 35min in thin film evaporator (9), obtains phosphate flame retardant
Through thin film evaporator discharge port (11) discharge thin film evaporator (9), distillation waste water enters condenser through distilling wastewater outlet (20)
(21) it is discharged afterwards；It obtains phosphate flame retardant to be filtered, completes last handling process.
The phosphate flame retardant 405.8kg that content is 96.5%, yield 95.5% are obtained, post-processing takes 2.5h altogether,
Waste water 185kg is generated, distillation process steam consumption is 11.2kg.
Embodiment 2
It is post-processed in the after-treatment device for the phosphate flame retardant that above-described embodiment 1 provides, the phosphate resistance
Combustion agent the after-treatment device course of work be specially：
(1) it is 100kg/h through delivery pump (13) control flow by 500kg phosphates crude product, then through caustic wash tower feed inlet (2)
Into caustic wash tower (1), while by a concentration of 5% sodium hydrate aqueous solution in alkali storage device (12) through delivery pump (14)
Control flow is 20kg/h, then enters caustic wash tower (1) through lye import (3), and the phosphate crude product and aqueous sodium carbonate are inverse
Stream contact 20min, carries out alkali cleaning, obtains the phosphate after alkali cleaning through caustic wash tower discharge port (4) discharge caustic wash tower (1), alkali cleaning is useless
Water is through alkali-wash waste water outlet (18) discharge caustic wash tower (1)；
(2) it is through delivery pump (15) control flow by the phosphate after the alkali cleaning being discharged by caustic wash tower discharge port (4)
100kg/h, then enter water scrubber (5) through water scrubber feed inlet (6), while being 30kg/ through delivery pump (16) control flow by water
H, then enter water scrubber (5), the phosphate after the alkali cleaning and water counter current contacting 30min through technique water inlet (7), carry out water
It washes, through water scrubber discharge port (8) discharge water scrubber (5), washing waste water exports the phosphate after being washed through washing waste water
(19) discharge water scrubber (5)；
(3) will be entered through thin film evaporator feed inlet (10) by the phosphate after the washing of water scrubber discharge port (8) discharge
Thin film evaporator (9), thin film evaporator (9) are passed through steam by steam inlet (22), and obtained condensed water is gone out by condensed water
Mouth (23) discharge；Phosphate after washing carries out thin film evaporation 30min in thin film evaporator (9), obtains phosphate flame retardant
Through thin film evaporator discharge port (11) discharge thin film evaporator (9), distillation waste water enters condenser through distilling wastewater outlet (20)
(21) it is discharged afterwards；It obtains phosphate flame retardant to be filtered, completes last handling process.
It is 96% phosphate flame retardant 402.3kg to obtain content, and yield 94.3% post-processes and takes 3.6h altogether, generates
Waste water 197.6kg, distillation process steam consumption are 10.5kg.
Embodiment 3
It is post-processed in the after-treatment device for the phosphate flame retardant that above-described embodiment 1 provides, the phosphate resistance
Combustion agent the after-treatment device course of work be specially：
(1) it is 100kg/h through delivery pump (13) control flow by 500kg phosphates crude product, then through caustic wash tower feed inlet (2)
Into caustic wash tower (1), while by a concentration of 15% potassium hydroxide aqueous solution in alkali storage device (12) through delivery pump
(14) control flow is 8kg/h, then enters caustic wash tower (1), the phosphate crude product and aqueous sodium carbonate through lye import (3)
Counter current contacting 7min carries out alkali cleaning, obtains the phosphate after alkali cleaning through caustic wash tower discharge port (4) discharge caustic wash tower (1), alkali cleaning is useless
Water is through alkali-wash waste water outlet (18) discharge caustic wash tower (1)；
(2) it is through delivery pump (15) control flow by the phosphate after the alkali cleaning being discharged by caustic wash tower discharge port (4)
100kg/h, then enter water scrubber (5) through water scrubber feed inlet (6), while being 50kg/ through delivery pump (16) control flow by water
H, then enter water scrubber (5), the phosphate after the alkali cleaning and water counter current contacting 8min through technique water inlet (7), it is washed,
Phosphate after being washed through water scrubber discharge port (8) discharge water scrubber (5), through washing waste water outlet (19) arrange by washing waste water
Go out water scrubber (5)；
(3) will be entered through thin film evaporator feed inlet (10) by the phosphate after the washing of water scrubber discharge port (8) discharge
Thin film evaporator (9), thin film evaporator (9) are passed through steam by steam inlet (22), and obtained condensed water is gone out by condensed water
Mouth (23) discharge；Phosphate after washing carries out thin film evaporation 30min in thin film evaporator (9), obtains phosphate flame retardant
Through thin film evaporator discharge port (11) discharge thin film evaporator (9), distillation waste water enters condenser through distilling wastewater outlet (20)
(21) it is discharged afterwards；It obtains phosphate flame retardant to be filtered, completes last handling process.
The phosphate flame retardant 406.9kg that content is 95.5%, yield 94.8% are obtained, post-processing takes 2.8h altogether,
Waste water 215kg is generated, distillation process steam consumption is 13.4kg.
Comparative example
The after-treatment device of the phosphate flame retardant provided using the prior art is post-processed, and the course of work is specially：
(1) the phosphate crude product 500kg that phosphate ester content is 82% is added into 1000L enamel stills, opens stirring, then
It is slowly added to the dilute sulfuric acid of 10kg a concentration of 70%, after reacting 1h, static layering 1h, upper layer obtains pickling waste waters 22kg, lower layer
Obtain the phosphate after 488kg pickling.
(2) phosphate after pickling is sent to alkali cleaning kettle, soda ash 10kg is added from alkali cleaning kettle man-hole opening, 50kg water is added,
Stirring and dissolving, after reacting 2h, static layering 1h, upper layer obtains alkali-wash waste water 95kg, and lower layer obtains the phosphate after alkali cleaning
453kg。
(3) phosphate after alkali cleaning is sent to washing kettle, 50kg water is added, after being stirred to react 1h, static layering 1h, upper layer
Obtain washing waste water 76kg, lower layer washed after phosphate 427kg.
(4) phosphate after washing is sent to distillation still, decompression dehydration, after being dehydrated 1.5h, filtering obtains organic phosphate flame-retardant
Agent.
The phosphate flame retardant 388kg that content is 95%, yield 89.9% are obtained, post-processing takes 8.5h altogether, generates
Waste water 232kg, distillation process steam consumption are 48.75kg.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest range.
Claims (9)
1. a kind of after-treatment device of phosphate flame retardant, which is characterized in that including：
Caustic wash tower for carrying out alkali cleaning to phosphate crude product, the caustic wash tower are equipped with feed inlet, lye import and discharge port；Institute
It is three (chloro isopropyl) phosphates, three (β-ethyl) phosphates, trimethyl phosphate, triethyl phosphate, phosphoric acid to state phosphate crude product
The crude product of three second propyl phenyl esters, bisphenol-A-(diphenyl phosphoester) or resorcinol-(double diphenyl phosphoesters)；The caustic wash tower
Alkali cleaning is carried out continuously to phosphate crude product, phosphate crude product carries out alkali cleaning with lye by counter current contacting；
The water scrubber that feed inlet is connected with the caustic wash tower discharge port, the water scrubber are equipped with technique water inlet and discharge port；
The water scrubber is carried out continuously washing to the phosphate after alkali cleaning, and the phosphate after alkali cleaning carries out water with water by counter current contacting
It washes；
The thin film evaporator that feed inlet is connected with the water scrubber discharge port, the thin film evaporator are equipped with discharge port, are used for
Output phosphate flame retardant；The thin film evaporator distills the phosphate after washing；
The caustic wash tower feed inlet, lye import, water scrubber feed inlet and technique water inlet are respectively arranged with volume control device.
2. after-treatment device according to claim 1, which is characterized in that further include：
Alkali storage device for preparing and storing lye；The alkali storage device is connected with the feed inlet of the caustic wash tower
It is logical.
3. after-treatment device according to claim 1, which is characterized in that further include：
Filter；The filter is connected with the discharge port of the thin film evaporator.
4. a kind of post-processing approach of phosphate flame retardant, which is characterized in that using after 3 any one of them of claims 1 to 3
Processing unit；The post-processing approach includes the following steps：
A) phosphate crude product and lye are subjected to the first counter current contacting, obtain the phosphate after alkali cleaning；
B) phosphate after alkali cleaning is subjected to the second counter current contacting, the phosphate after being washed with water；
C) phosphate after washing is subjected to thin film evaporation, obtains phosphate flame retardant.
5. post-processing approach according to claim 4, which is characterized in that the lye is aqueous sodium carbonate, hydroxide
It is one or more in sodium water solution and potassium hydroxide aqueous solution.
6. post-processing approach according to claim 4, which is characterized in that a concentration of the 5%~15% of the lye.
7. post-processing approach according to claim 4, which is characterized in that the first counter current contacting process described in step a)
In, the flow-rate ratio of the flow of the lye and the phosphate crude product is (8~25)：100；The time of first counter current contacting
For 7min~20min.
8. post-processing approach according to claim 4, which is characterized in that the second counter current contacting process described in step b)
In, the flow-rate ratio of the flow of the water and the phosphate after the alkali cleaning is (20~50)：100；Second counter current contacting
Time is 8min~30min.
9. post-processing approach according to claim 4, which is characterized in that the step c) further includes：
Phosphate after thin film evaporation is filtered.
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| CN114478620B (en) * | 2022-02-23 | 2024-03-22 | 淮安晨化新材料有限公司 | Preparation process of odorless phosphate flame retardant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887917A (en) * | 2011-10-14 | 2013-01-23 | 江苏大明科技有限公司 | Preparation method of TCPP (trichloropropylphosphate) flame retardant |
| CN103570759A (en) * | 2012-07-26 | 2014-02-12 | 中国石油天然气股份有限公司 | Continuous alkali washing method of resorcinol bis (di-2, 6-dimethylphenyl phosphate) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887917A (en) * | 2011-10-14 | 2013-01-23 | 江苏大明科技有限公司 | Preparation method of TCPP (trichloropropylphosphate) flame retardant |
| CN103570759A (en) * | 2012-07-26 | 2014-02-12 | 中国石油天然气股份有限公司 | Continuous alkali washing method of resorcinol bis (di-2, 6-dimethylphenyl phosphate) |
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