CN214991242U - Production facility of phosphonate aluminum salt fire retardant - Google Patents

Production facility of phosphonate aluminum salt fire retardant Download PDF

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CN214991242U
CN214991242U CN202120602229.8U CN202120602229U CN214991242U CN 214991242 U CN214991242 U CN 214991242U CN 202120602229 U CN202120602229 U CN 202120602229U CN 214991242 U CN214991242 U CN 214991242U
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reaction kettle
storage tank
kettle
pipeline
flame retardant
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孙素丽
吕从高
周明
刘玉荣
张润茹
颜家力
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Honghu Yitai Technology Co ltd
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Honghu Yitai Technology Co ltd
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Abstract

The utility model provides a production device of aluminum phosphonate flame retardant, which comprises a first reaction kettle, a double-cone dryer, a second reaction kettle, a first distillation kettle, a first drying filter, a third reaction kettle and a second drying filter which are connected in sequence through pipelines, the material generated by the heating reaction in the first reaction kettle is conveyed to a double-cone dryer for drying, the dried material is conveyed to a second reaction kettle for heating reaction, the material generated in the second reaction kettle is conveyed to the first distillation kettle for distillation, the material in the first distillation kettle is conveyed to the first drying filter for filtration and drying, and conveying the material in the first dry filter to a third reaction kettle for heating reaction, and conveying the material generated in the third reaction kettle to a second dry filter for filtering and drying to obtain the aluminum phosphonate flame retardant.

Description

Production facility of phosphonate aluminum salt fire retardant
Technical Field
The utility model relates to a fire retardant technical field especially relates to a production facility of phosphonate aluminium salt fire retardant.
Background
The flame retardant is a functional auxiliary agent for endowing inflammable polymers with flame retardancy, is mainly designed aiming at the flame retardancy of high polymer materials, is applied to the fields of transportation, electronic and electrical equipment, furniture and building materials, and can reduce the occurrence of fire.
The halogen-containing flame retardant is a flame retardant product with the most flame-retardant application in high polymer materials, has good compatibility with plastics, good flame-retardant effect and low use cost, has large smoke generation amount when the halogen flame retardant is combusted, releases a large amount of highly corrosive hydrogen halide gas and other toxic and harmful substances, and is easy to cause secondary harm and environmental pollution; in recent years, phosphorus flame retardants gradually become popular to replace halogen-containing flame retardants, and have the advantages of easy preparation, good flame retardant property and good thermal stability, however, with the progress of research, single-element flame retardance cannot meet production requirements, and multiple-element synergistic flame retardance can make up for the deficiency of single flame retardance and improve the flame retardant property, so that the development of equipment suitable for producing multiple-element synergistic flame retardants is particularly important.
Disclosure of Invention
In view of this, the utility model provides a production facility of phosphonate aluminium salt fire retardant.
The utility model provides a production facility of aluminium phosphonate fire retardant, include the first reation kettle, bipyramid desicator, second reation kettle, first stills, first drier, third reation kettle and the second drier that connect gradually through the pipeline, first reation kettle connects diethyl methylphosphonite holding vessel, phenylacrylamide holding vessel, ethyl acetate holding vessel and glacial acetic acid holding vessel, the second reation kettle connects the sulphuric acid solution holding vessel, first stills and third reation kettle all connect the isopropyl alcohol holding vessel, the third reation kettle still connects isopropyl alcohol-aluminium isopropoxide holding vessel, the material that produces of heating reaction in the first reation kettle is carried to bipyramid desicator and is dried, and the material after the drying is carried to the second reation kettle and carries out the heating reaction, the material that produces in the second reation kettle is carried to first stills and is distilled, and conveying the material in the first distillation kettle to a first drying filter for filtering and drying, conveying the material in the first drying filter to a third reaction kettle for heating reaction, and conveying the material generated in the third reaction kettle to a second drying filter for filtering and drying to obtain the aluminum phosphonate flame retardant.
Further, a second discharge port is formed in the first reaction kettle, a fourth discharge port is formed in the double-cone dryer, the second discharge port and the fourth discharge port are connected with an ethyl acetate recovery tank through pipelines, and the ethyl acetate recovery tank stores recovered ethyl acetate.
Further, a sixth discharge hole is formed in the first distillation kettle and connected with an ethanol recovery tank through a pipeline, and the ethanol recovery tank stores recovered ethanol.
Further, first drier-filter and second drier-filter all connect second stills, set up the tenth discharge gate on the second stills, the tenth discharge gate passes through the pipeline and is connected with the isopropyl alcohol holding vessel.
Further, set up first feed inlet, second feed inlet and third feed inlet on the first reation kettle, first feed inlet passes through the pipeline and is connected with the diethyl methylphosphonite holding vessel, the second feed inlet passes through the pipeline and is connected with the phenylacrylamide holding vessel, the third feed inlet passes through the pipeline and is connected with ethyl acetate holding vessel and glacial acetic acid holding vessel.
Further, a fifth feed inlet is formed in the second reaction kettle and connected with a sulfuric acid solution storage tank through a pipeline.
Further, an eighth feed inlet is formed in the first distillation kettle and connected with an isopropanol storage tank through a pipeline.
Further, an eleventh feeding hole and a twelfth feeding hole are formed in the third reaction kettle, the eleventh feeding hole is connected with the isopropanol storage tank through a pipeline, and the twelfth feeding hole is connected with the isopropanol-aluminum isopropoxide storage tank through a pipeline.
The utility model provides a beneficial effect that technical scheme brought is: the utility model provides a production facility uses phenyl acrylamide, diethyl methylphosphonite and aluminium isopropoxide to make aluminium phosphonate fire retardant as the raw materials, and simple process is fit for extensive industrial production, and in the production process isopropanol, ethyl acetate can be retrieved and apply mechanically, have effectively improved the utilization ratio of raw materials.
Drawings
FIG. 1 is a schematic structural diagram of a production facility for aluminum phosphonate flame retardant of the present invention.
FIG. 2 is a reaction mechanism diagram for preparing an aluminum phosphonate flame retardant in an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, embodiments of the present invention will be further described below with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides a production apparatus for an aluminum phosphonate flame retardant, including a first reaction kettle 1, a double-cone dryer 2, a second reaction kettle 3, a first distillation kettle 4, a first drying filter 5, a third reaction kettle 6, and a second drying filter 7, which are connected in sequence through a pipeline.
First reation kettle 1 is last to set up first feed inlet 11, second feed inlet 12, third feed inlet 13, first discharge gate 14 and second discharge gate 15, first feed inlet 11 passes through the pipeline and is connected with diethyl methylphosphonite holding vessel 16, second feed inlet 12 passes through the pipeline and is connected with phenylacrylamide holding vessel 17, third feed inlet 13 passes through the pipeline and is connected with ethyl acetate holding vessel 18 and glacial acetic acid holding vessel 19, store diethyl methylphosphonite in diethyl methylphosphonite holding vessel 16, store phenylacrylamide in phenylacrylamide holding vessel 17, store ethyl acetate in ethyl acetate holding vessel 18, store glacial acetic acid in glacial acetic acid holding vessel 19, second discharge gate 15 passes through the pipeline and is connected with ethyl acetate recovery tank 151, ethyl acetate recovery tank 151 is used for storing the ethyl acetate of retrieving.
The double-cone dryer 2 is provided with a fourth feeding hole 21, a third discharging hole 22 and a fourth discharging hole 23, the fourth feeding hole 21 is connected with the first discharging hole 14 through a pipeline, and the third discharging hole 22 is connected with the ethyl acetate recovery tank 151 through a pipeline.
The second reaction kettle 3 is provided with a fifth feeding hole 31, a sixth feeding hole 32 and a fifth discharging hole 33, the fifth feeding hole 31 is connected with a sulfuric acid solution storage tank 34 through a pipeline, the sixth feeding hole 32 is connected with the fourth discharging hole 23 through a pipeline, and the sulfuric acid solution is stored in the sulfuric acid solution storage tank 34.
Set up seventh feed inlet 41, eighth feed inlet 42, sixth discharge gate 43 and seventh discharge gate 44 on first stills 4, seventh feed inlet 41 passes through the pipeline to be connected with fifth discharge gate 33, and eighth feed inlet 42 passes through the pipeline to be connected with isopropyl alcohol holding vessel 45, and sixth discharge gate 43 passes through the pipeline to be connected with ethanol recovery tank 46, and isopropyl alcohol holding vessel 45 is used for storing isopropyl alcohol, and ethanol recovery tank 46 is used for storing the ethanol of retrieving.
The first drying filter 5 is provided with a ninth feeding hole 51, an eighth discharging hole 52 and a ninth discharging hole 53, the ninth feeding hole 51 is connected with the seventh discharging hole 44 through a pipeline, the eighth discharging hole 52 is connected with the second distillation kettle 54 through a pipeline, the second distillation kettle 54 is provided with a tenth discharging hole 541, and the tenth discharging hole 541 is connected with the isopropanol storage tank 45 through a pipeline.
The third reaction kettle 6 is provided with a tenth material port 61, an eleventh material port 62, a twelfth material port 63 and an eleventh material port 64, the tenth material port 61 is connected with the ninth material port 53 through a pipeline, the eleventh material port 62 is connected with the isopropanol storage tank 45 through a pipeline, the twelfth material port 63 is connected with the isopropanol-aluminum isopropoxide storage tank 65 through a pipeline, and isopropanol solution of aluminum isopropoxide is stored in the isopropanol-aluminum isopropoxide storage tank 65.
The second dry filter 7 is provided with a thirteenth feeding hole 71, a twelfth discharging hole 72 and a thirteenth discharging hole 73, the thirteenth feeding hole 71 is connected with the eleventh discharging hole 64 through a pipeline, the twelfth discharging hole 72 is connected with the second distillation kettle 54 through a pipeline, and a product generated in the second dry filter 7 is discharged from the thirteenth discharging hole 73.
And the first drying filter 5 and the second drying filter 7 are all integrated machines of filtering, washing and drying.
In one embodiment, the process for producing the aluminum phosphonate flame retardant by using the production equipment comprises the following steps: adding 1.47 tons of phenylacrylamide (compound 2) stored in a phenylacrylamide storage tank 17 into a first reaction kettle 1, then adding 2 tons of ethyl acetate stored in an ethyl acetate storage tank 18 and 600kg of glacial acetic acid stored in a glacial acetic acid storage tank 19 into the first reaction kettle 1, adding 3.4 tons of diethyl methylphosphonite (compound 1) stored in a diethyl methylphosphonite storage tank 16 into the first reaction kettle 1 under the conditions of nitrogen protection and the kettle temperature of the first reaction kettle 1 of 50 ℃, keeping the temperature in the first reaction kettle 1 not more than 70 ℃, stirring for reaction for 2 hours, cooling to room temperature after the reaction is finished, slowly heating to 50 ℃ at-3.5 KPa, evaporating the ethyl acetate and the excessive diethyl methylphosphonite, and allowing the ethyl acetate and the excessive diethyl methylphosphonite to enter an ethyl acetate recovery tank through a second discharge port 15, when the system in the first reaction kettle 1 is in a slurry state, nitrogen is used for pressing the slurry material into a double-cone dryer 2, the system is completely evaporated at minus 3.5KPa and 70 ℃, and the recovered ethyl acetate and diethyl methylphosphonite enter an ethyl acetate recovery tank 151 through a third discharge port 22;
adding a sulfuric acid solution in a sulfuric acid solution storage tank 34 into a second reaction kettle 3 through a fifth feeding hole 31, then conveying 2.55 tons of light brown red solid powder (compound 3) generated in a double-cone dryer 2 into the second reaction kettle 3 through a fourth discharging hole 23 and a sixth feeding hole 32 under the stirring condition, heating to 100-110 ℃ for reaction for 4 hours while stirring, then adding materials in the second reaction kettle 3 into a first distillation kettle 4 through a fifth discharging hole 33 and a seventh feeding hole 41, gradually heating to 100 ℃ under-3.5 KPa to distill off water and by-product ethanol, introducing the distilled water and ethanol into an ethanol recovery tank 46 through a sixth discharging hole 43, adding 2 tons of isopropanol into the first distillation kettle 4 from an isopropanol storage tank 45, cooling the reaction system in the first distillation kettle 4 to 0 ℃, stirring for 30 minutes, and then conveying the reaction system in the first distillation kettle 4 to a first drying device through a seventh discharging hole 44 and a ninth feeding hole 51 by using a conveying pump A filter 5, wherein filtrate generated by filtration enters a second distillation kettle 54 through an eighth discharge hole 52, filter cakes generated by filtration are washed by 500kg of isopropanol, the filtrate generated by washing is sent to the second distillation kettle 54, the temperature of the isopropanol in the second distillation kettle 54 is gradually increased to 60 ℃ at minus 3.5KPa, the distilled isopropanol and the isopropanol in the filter cake in the first drying filter 5 are sent to an isopropanol storage tank 45 together after being dried in vacuum for 2 hours at minus 3.5KPa and 60 ℃ and are used for reaction and washing processes; discharging the first dry filter 5 to obtain white solid powder (compound 4);
pumping 400kg of isopropanol into the third reaction kettle 6 from an isopropanol storage tank 45, conveying 454kg of white solid powder in the first drying filter 5 to the third reaction kettle 6 through a ninth discharge port 53 and a tenth discharge port 61 under stirring, heating a reaction system in the third reaction kettle 6 to 40 ℃, stirring for 30min to fully dissolve the white solid powder, then pumping 100kg of isopropanol solution of aluminum isopropoxide (containing 13.6kg of aluminum isopropoxide) prepared in advance into the third reaction kettle 6 within 1h at a certain flow rate from an isopropanol-aluminum isopropoxide storage tank 65, stirring and refluxing for 1h after the addition is finished, cooling to room temperature after the reaction is finished, then conveying materials in the third reaction kettle 6 to the second drying filter 7 through a thirteenth feed port 71 and an eleventh discharge port 64, filtering to obtain filtrate, and conveying the filtrate into the second distillation kettle 54 through a twelfth discharge port 72, washing the filter cake with 100kg of isopropanol, feeding the filtrate generated by washing into a second distillation kettle 54, distilling the second distillation kettle 54 at-3.5 KPa and 60 ℃, feeding the distilled isopropanol and the isopropanol distilled out from the filter cake in a second drying filter 7 after vacuum drying for 2 hours at-3.5 KPa and 60 ℃ into an isopropanol storage tank 45, and applying the isopropanol and the filter cake in the second drying filter 7 for reaction and washing, wherein the white powder solid left in the second drying filter 7 is the aluminium phosphonate flame retardant (marked as a compound YT002), and the reaction mechanism of the production process is shown in figure 2.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.

Claims (8)

1. Production equipment of aluminum phosphonate flame retardant is characterized by comprising a first reaction kettle, a double-cone dryer, a second reaction kettle, a first distillation kettle, a first drying filter, a third reaction kettle and a second drying filter which are sequentially connected through pipelines, wherein the first reaction kettle is connected with a diethyl methylphosphonite storage tank, a phenylacrylamide storage tank, an ethyl acetate storage tank and a glacial acetic acid storage tank, the second reaction kettle is connected with a sulfuric acid solution storage tank, the first distillation kettle and the third reaction kettle are both connected with an isopropanol storage tank, the third reaction kettle is also connected with an isopropanol-aluminum isopropoxide storage tank, a material generated by heating reaction in the first reaction kettle is conveyed to the double-cone dryer for drying, the dried material is conveyed to the second reaction kettle for heating reaction, a material generated in the second reaction kettle is conveyed to the first distillation kettle for distillation, and conveying the material in the first distillation kettle to a first drying filter for filtering and drying, conveying the material in the first drying filter to a third reaction kettle for heating reaction, and conveying the material generated in the third reaction kettle to a second drying filter for filtering and drying to obtain the aluminum phosphonate flame retardant.
2. The apparatus for producing an aluminum phosphonate flame retardant of claim 1, wherein the first reaction kettle is provided with a second discharge port, the double-cone dryer is provided with a fourth discharge port, the second discharge port and the fourth discharge port are both connected with an ethyl acetate recovery tank through pipelines, and the ethyl acetate recovery tank stores recovered ethyl acetate.
3. The apparatus for producing aluminum phosphonate flame retardant of claim 1, wherein the first distillation still is provided with a sixth discharge port, the sixth discharge port is connected with an ethanol recovery tank through a pipeline, and the ethanol recovery tank stores recovered ethanol.
4. The production equipment of the aluminum phosphonate flame retardant of claim 1, wherein the first drying filter and the second drying filter are both connected to a second distillation kettle, a tenth discharge port is arranged on the second distillation kettle, and the tenth discharge port is connected to an isopropanol storage tank through a pipeline.
5. The aluminum phosphonate flame retardant production equipment of claim 1, wherein the first reaction kettle is provided with a first feed port, a second feed port and a third feed port, the first feed port is connected with a diethyl methylphosphonite storage tank through a pipeline, the second feed port is connected with a phenylacrylamide storage tank through a pipeline, and the third feed port is connected with an ethyl acetate storage tank and a glacial acetic acid storage tank through pipelines.
6. The aluminum phosphonate flame retardant production facility of claim 1, wherein the second reaction kettle is provided with a fifth feed inlet, and the fifth feed inlet is connected with a sulfuric acid solution storage tank through a pipeline.
7. The aluminum phosphonate flame retardant production facility of claim 1, wherein the first distillation still is provided with an eighth feed inlet, and the eighth feed inlet is connected with an isopropanol storage tank through a pipeline.
8. The aluminum phosphonate flame retardant production equipment of claim 1, wherein the third reaction kettle is provided with an eleventh feed inlet and a twelfth feed inlet, the eleventh feed inlet is connected with an isopropanol storage tank through a pipeline, and the twelfth feed inlet is connected with an isopropanol-aluminum isopropoxide storage tank through a pipeline.
CN202120602229.8U 2021-03-24 2021-03-24 Production facility of phosphonate aluminum salt fire retardant Active CN214991242U (en)

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Application Number Priority Date Filing Date Title
CN202120602229.8U CN214991242U (en) 2021-03-24 2021-03-24 Production facility of phosphonate aluminum salt fire retardant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202120602229.8U CN214991242U (en) 2021-03-24 2021-03-24 Production facility of phosphonate aluminum salt fire retardant

Publications (1)

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CN214991242U true CN214991242U (en) 2021-12-03

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