CN114470605B - Treatment method and treatment system for alkyl aluminum hazardous waste - Google Patents
Treatment method and treatment system for alkyl aluminum hazardous waste Download PDFInfo
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- CN114470605B CN114470605B CN202011170767.0A CN202011170767A CN114470605B CN 114470605 B CN114470605 B CN 114470605B CN 202011170767 A CN202011170767 A CN 202011170767A CN 114470605 B CN114470605 B CN 114470605B
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Abstract
The invention discloses a method and a system for treating alkyl aluminum hazardous waste, wherein the method comprises the following steps: (1) Diluting the aluminum alkyl hazardous waste by using an inert organic solvent to obtain a diluent; (2) Injecting the diluent into water, stirring and hydrolyzing to obtain hydrolysate; (3) And adding an acidic medium into the hydrolysate, and stirring for acidolysis treatment to obtain a mixed solution with stable performance. In the method, the alkyl aluminum hazardous waste is diluted by the organic solvent, so that the danger of the process is reduced; the reaction heat release in the hydrolysis process is controlled by controlling the injection speed, so that the safety coefficient is greatly improved; the solid content in the hydrolysis waste liquid is reduced through the acidolysis process, the formation of an emulsion in the waste liquid is reduced, and the efficiency of diluting the solvent and recovering water is greatly improved.
Description
Technical Field
The invention relates to the field of chemical hazardous waste treatment, in particular to a method and a system for treating alkyl aluminum hazardous waste.
Background
The alkylaluminum is an organic compound containing a metal aluminum in which an alkyl group is directly bonded to aluminum, and is also called trialkylaluminum. Aluminum alkyls are used in large quantities for the preparation of catalysts for Ziegler-Natta reactions and are used as intermediates in organic synthesis. But the chemical property of the alkyl aluminum is very active, for example, triethyl aluminum can be spontaneously combusted in air, is very easy to be oxidized and explodes when meeting water, and has higher hazard.
The treatment of the hazardous waste of the aluminum alkyl is always a safety key and a difficulty in the relevant synthesis production. At present, the aluminum alkyl hazardous waste is treated by mainly adopting a destroying method. Due to the chemical nature of aluminum alkyls, which are very reactive, great care must be taken in the destruction process for safety reasons.
CN201110446763.5 proposes a recovery processing method of hazardous waste in the production process of alkyl aluminum. The method comprises the steps of replacing a reaction kettle with nitrogen, adding a solvent containing aluminum alkyl and aluminum powder into the reaction kettle, introducing carbon dioxide for passivation, adding 50-300 vol% of water based on the volume of the solvent, and controlling the reaction temperature to be 10-60 ℃ and the pressure in the reaction process to be 0.01-0.1 MPa to complete the hydrolysis process. However, this method does not notice that the reaction of water with aluminum alkyl is very rapid and violent, and introduction of water into an organic solvent containing aluminum alkyl is liable to cause local overheating, and the solvent has a high possibility of temperature runaway.
CN201010117603.1 proposes a method to remove residual aluminum alkyl from waste. The aluminum alkyl is reacted by adding water and polyaluminum chloride to a paraffin solution in which the aluminum alkyl is dissolved. The method needs 60-240 hours for adding water, strictly controls the temperature to be 10-60 ℃ in the reaction process, and has extremely strict requirements on a control system.
In conclusion, the existing treatment method for the aluminum alkyl hazardous waste has the problems of complex flow, high difficulty of the control method, poor process safety and the like.
Disclosure of Invention
The invention aims to solve the problems of complex flow, high difficulty of a control method, poor process safety and the like of a treatment method of aluminum alkyl hazardous waste in the prior art, and provides a treatment method and a treatment system of the aluminum alkyl hazardous waste.
One of the purposes of the invention is to provide a method for treating aluminum alkyl hazardous waste, wherein the method comprises the following steps:
(1) Diluting the aluminum alkyl hazardous waste by using an inert organic solvent to obtain a diluent;
(2) Injecting the diluent into water, stirring and hydrolyzing to obtain hydrolysate;
(3) And adding an acidic medium into the hydrolysate, and stirring for acidolysis treatment to obtain a mixed solution with stable performance.
The invention aims at the alkyl aluminum hazardous waste with higher concentration, and preferably carries out dilution before the alkyl aluminum hazardous waste is treated, and then hydrolyzes to eliminate active components in the alkyl aluminum hazardous waste.
In the present invention, the alkylaluminum is selected from triethylaluminum, triisobutylaluminum, triisopropylaluminum, diethylaluminum chloride, ethylaluminum dichloride, pentyldicyclohexylaluminum, and at least one of methylaluminum and methoxyaluminum.
Among them, alkylaluminums are extremely flammable, have strong corrosivity and irritation, have high chemical reaction activity, and can smoke and spontaneously combust when contacting air. The reaction is very sensitive to micro-oxygen-based water, and the combustion and explosion are easy to cause. In the prior art, the treatment of waste aluminum alkyl (such as triethyl aluminum) is to add an ATMER163 to inactivate triethyl aluminum, the waste aluminum alkyl is added with the ATMER163 and then is pressed into a storage tank by nitrogen, and then is sent to an oil sludge storage of a special waste fluidized bed combustion furnace for subsequent treatment.
In the method, the alkyl aluminum hazardous waste is diluted by the organic solvent, so that the danger of the process is reduced; meanwhile, the reaction heat release in the hydrolysis process is controlled by controlling the injection speed, so that the safety coefficient is greatly improved.
In a preferred embodiment, in step (1), the inert organic solvent is selected from organic solvents that do not react with water.
In a further preferred embodiment, in step (1), the inert organic solvent is selected from at least one of toluene, hexane, petroleum ether, benzene, octane, preferably from toluene and/or hexane.
In a further preferred embodiment, the dilution in step (1) contains less than 10wt%, preferably less than 5wt%, and more preferably less than 2wt% of the aluminum alkyl hazardous waste.
In a preferred embodiment, in step (1), the alkylaluminum hazardous waste is injected into the inert organic solvent.
In a further preferred embodiment, in step (1), the injection amount per minute is not more than 40% of the total amount of the aluminum alkyl hazardous waste, preferably not more than 30% of the total amount of the aluminum alkyl hazardous waste, and more preferably not more than 20% of the total amount of the aluminum alkyl hazardous waste.
In a preferred embodiment, the dilution in step (1) is carried out at a temperature below 45 ℃.
In a further preferred embodiment, the dilution in step (1) is carried out in a vessel having a stirring function and a cooling function, or in a vessel having a bubbling nitrogen function and a cooling function.
In the invention, the alkyl aluminum hazardous waste is diluted by the organic solvent, so that the danger of the process is reduced.
In a preferred embodiment, in step (2), the injection amount per minute is not more than 15% of the total weight of the diluent.
In a further preferred embodiment, in step (2), the amount injected per minute is not more than 10% of the total weight of the diluent, preferably not more than 5% of the total weight of the diluent.
Wherein, the reaction heat release in the hydrolysis process is controlled by controlling the injection speed, and the safety factor is greatly improved
In a preferred embodiment, in step (2), the weight ratio of the total amount of water to the dilution obtained in step (1) is 1:3 or more, preferably 1:1 or more, more preferably 3:1 or more.
In a preferred embodiment, the hydrolysis of step (2) is carried out at a temperature below 45 ℃.
In a further preferred embodiment, the hydrolysis of step (2) is carried out at 35-45 ℃.
In a further preferred embodiment, the hydrolysis in step (2) is carried out in a vessel having a stirring function and a cooling function, or in a vessel having a drum nitrogen function and a cooling function.
Wherein, the hydrolysis treatment process releases a large amount of heat and needs to be carried out under the stirring and cooling effects, and the cooling process is carried out at the temperature below 45 ℃. The circulating water is used as a cooling medium, and the temperature control process is simple.
In a preferred embodiment, a gas-phase product is generated in the hydrolysis process in the step (2), and the gas-phase product is introduced into a water washing tower to be washed by water and then discharged out of a battery limit.
In a further preferred embodiment, the number of theoretical plates of the water wash column is from 1 to 5, the operating pressure is from 0.01 to 0.60MPag, the temperature at the top of the column is from 25 to 45 ℃ and the temperature at the bottom of the column is from 35 to 46 ℃.
Wherein the number of theoretical plates of the water washing tower is 2, 3, 4 or 5; the operating pressure is 0.05MPag, 0.1MPag, 0.2MPag, 0.3MPag, 0.4MPag, 0.5MPag or 0.6MPag; the temperature at the top of the tower is 25 ℃, 30 ℃, 35 ℃, 40 ℃ or 45 ℃; the temperature of the tower bottom is 35 ℃, 40 ℃ or 46 ℃.
In a further preferred embodiment, a portion of the water in the water wash column is periodically drained and replaced with a portion of the water. Preferably, the discharged water is used as the hydrolysis water in the step (2), so that the system wastewater discharge is reduced.
Wherein, the washing tower runs for a long time, and the inside circulating water and oil can form emulsion, so need regularly to discharge partly water, and supply partly water and replace.
In a preferred embodiment, in step (3), the acidic medium is selected from mineral acids, preferably from at least one of hydrochloric acid, nitric acid and sulfuric acid, more preferably from hydrochloric acid and/or sulfuric acid.
The acidolysis treatment refers to adding an acidic medium after the hydrolysis process to acidolyze an emulsion generated by an organic inert solvent and water, and simultaneously neutralizing products with low solubility in water such as aluminum hydroxide and the like generated in the hydrolysis process, wherein the acidic medium refers to inorganic acid substances such as hydrochloric acid or sulfuric acid and the like.
In a further preferred embodiment, the molar ratio of hydrogen ions to the aluminum alkyl in the acidic medium is (1-10): 1, preferably (2-6): 1, more preferably (3-6): 1.
Wherein the molar amount of the acidic medium is based on the molar amount of hydrogen ions therein.
In the invention, the solid content in the hydrolysis waste liquid is reduced through the acidolysis process, the formation of emulsion in the waste liquid is reduced, and the recovery efficiency of the diluting solvent and water is greatly improved.
In a preferred embodiment, step (4) and step (5) are performed after step (3):
(4) And filtering and standing the mixed solution to obtain an oil phase and a water phase.
(5) And (3) recovering the solvent from the obtained oil phase, discharging a part of the obtained water phase, and recycling the residual water phase as the hydrolysis water in the step (2).
Wherein the standing treatment refers to standing the mixed solution after acidolysis to separate an oil phase and a water phase. The water phase is recycled as hydrolysis water, and a part of wastewater is discharged in order to prevent salt substances generated in the hydrolysis process from precipitating due to overhigh concentration.
According to the method of the present invention, in the step (2), the water to be injected into the process is not particularly required, and it is preferable to use waste water produced in the system, such as waste water produced in a standing and water-washing tower, for hydrolysis.
In a preferred embodiment, the solvent recovery in step (5) is carried out in a solvent recovery tower, the oil-containing water phase (S9 waste liquid) in the tower bottom is discharged from a battery limit, and the oil phase obtained at the tower top is recycled as the diluent in step (1).
In a further preferred embodiment, the theoretical plate number of the solvent recovery column is 5 to 20 pieces, the operating pressure is 0.01 to 0.60MPag, the overhead temperature is 25 to 100 ℃ and the column bottom temperature is 45 to 250 ℃.
In a further preferred embodiment, the oil phase obtained at the top of the solvent recovery column is dried and recycled as diluent, preferably, the water content of the dried diluent solvent is controlled to be less than 500ppm, preferably less than 100ppm, more preferably less than 10ppm.
Wherein the circulating diluent is dehydrated, for example, by placing a molecular sieve in a drying tower. The recovered diluting solvent is dried, so that the risk of violent uncontrollable hydrolysis reaction in the diluting process is eliminated.
In a preferred embodiment, steps (1) to (5) are performed in an oxygen-free environment, preferably steps (1) to (3) are performed in an oxygen-free environment.
The other purpose of the invention is to provide a system for treating the alkyl aluminum hazardous waste, which is preferably used for carrying out the method of the first purpose, wherein the system comprises a dilution unit, a hydrolysis unit, a filtering unit and a standing unit which are connected in sequence.
In a preferred embodiment, the dilution unit comprises a container with stirring and cooling functions, such as a dilution tank.
In a preferred embodiment, the hydrolysis unit comprises a vessel with stirring and cooling functions, such as a hydrolysis kettle.
In a further preferred embodiment, a water tank and an acidic medium tank are arranged above the hydrolysis unit.
In a preferred embodiment, the system further comprises a water wash column connected to the gas phase outlet of the hydrolysis unit.
In a further preferred embodiment, the number of theoretical plates of the water wash column is from 1 to 5, the operating pressure is from 0.01 to 0.60MPag, the temperature at the top of the column is from 25 to 45 ℃ and the temperature at the bottom of the column is from 35 to 46 ℃.
In a further preferred embodiment, a make-up water inlet and a replacement water outlet are provided on the water wash column, the replacement water outlet optionally being connected to the water tank.
In a preferred embodiment, the filtration unit comprises a filter and the resting unit comprises a resting tank.
In a further preferred embodiment, the resting unit comprises an oil phase outlet and an aqueous phase outlet, wherein the aqueous phase outlet is optionally connected to the water tank.
In a preferred embodiment, the system further comprises a solvent recovery column and a drying column, wherein the solvent recovery column is connected with the oil phase outlet of the standing unit, and the drying column is connected with the top of the solvent recovery column.
In a further preferred embodiment, the theoretical plate number of the solvent recovery column is 5 to 20 pieces, the operating pressure is 0.01 to 0.60MPag, the overhead temperature is 25 to 100 ℃ and the column bottom temperature is 45 to 250 ℃.
In a preferred embodiment, the gas outlet of the drying column is connected to a dilution unit.
In a further preferred embodiment, a solvent recovery tank is provided between the top of the solvent recovery column and the drying column.
In a preferred embodiment, the system of the present invention operates in an anaerobic environment.
The endpoints of the ranges and any values disclosed in the present application are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein. In the following, various technical solutions can in principle be combined with each other to obtain new technical solutions, which should also be regarded as specifically disclosed herein.
Compared with the prior art, the invention has the following beneficial effects:
(1) In the method, the alkyl aluminum hazardous waste is diluted by the organic solvent, so that the danger of the technical process is reduced;
(2) In the method, the reaction heat release in the hydrolysis process is controlled by controlling the injection speed, so that the safety coefficient is greatly improved;
(3) In the method, the solid content in the hydrolysis waste liquid is reduced through the acidolysis process, the formation of an emulsion in the waste liquid is reduced, and the recovery efficiency of the diluting solvent and water is greatly improved;
(4) In the method, the temperature control range in the hydrolysis process is below 45 ℃, circulating water is used as a cooling medium, and the temperature control process is simple;
(5) In the method, the recovered diluting solvent is dried, so that the risk of violent uncontrollable hydrolysis reaction in the diluting process is eliminated.
Drawings
Fig. 1 shows a schematic of the system of the present invention.
Description of reference numerals:
a V1 dilution unit; a V2 water tank; a V3 acid medium tank; a V4 standing unit; a V5 solvent recovery storage tank; t1, washing a tower with water; a T2 solvent recovery column; t3, a drying tower; an R1 hydrolysis unit; an SR1 filtering unit; s1, alkyl aluminum hazardous waste; s2, inert organic solvent; s3, hydrolyzing and supplementing water; s4, an acidic medium; s5, washing with water to supplement water; s6, oil phase; s7, waste water; s8, waste gas; s9, waste liquor; s10, replacing water.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
It is to be further understood that the various features described in the following detailed description may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention can be made, as long as the technical solution formed by the combination does not depart from the idea of the present invention, and the technical solution formed by the combination is part of the original disclosure of the present specification, and also falls into the protection scope of the present invention.
The raw materials used in the examples and comparative examples are disclosed in the prior art if not particularly limited, and may be, for example, directly purchased or prepared according to the preparation methods disclosed in the prior art.
The composition of the aluminum alkyl hazardous waste used in the examples is shown in table 1.
Table 1:
| total amount of | 100kg |
| Components | The content is wt% |
| Trimethylaluminum | 11.5 |
| Toluene | 53.2 |
| Hexane (C) | 35.3 |
[ example 1 ]
The alkyl aluminum hazardous waste shown in the table 1 is treated by adopting the device shown in the figure 1.
V1 dilution tank; a V2 water tank; a V3 acid medium tank; v4, standing in a tank; v5 solvent recovery storage tank; t1, washing a tower with water; a T2 solvent recovery column; t3, a drying tower; r1 hydrolysis kettle; an SR1 filter; s1, alkyl aluminum hazardous waste; s2, inert organic solvent; s3, hydrolyzing and supplementing water; s4, an acidic medium; s5, washing with water to supplement water; s6, oil phase; s7, waste water; s8, waste gas; s9, waste liquor; s10, replacing water.
(1) In the dilution tank, 500kg of toluene was preset, the alkylaluminum hazardous wastes were injected at a rate of 20kg/min and mixed by nitrogen blowing while cooling by circulating water through the jacket, the maximum temperature in the tank was not higher than 35 ℃, and the trimethylaluminum content in the alkylaluminum dilute solution was 1.92% by weight.
(2) 2000kg of water was introduced into the hydrolysis kettle, the stirring was started, and circulating water was introduced into the jacket. The dilute solution of aluminum alkyl is injected into the hydrolysis kettle at a speed of 30 kg/min.
(3) The hydrolysis process was continued for 20min with stirring and cooling, the maximum temperature of the hydrolysis kettle was 36.7 ℃.
(4) The gas phase product obtained in the hydrolysis process enters a water washing tower for water washing treatment and then is discharged out of a boundary area, the number of theoretical plates of the water washing tower is 3, the operation pressure is 0.05MPag, the temperature of the top of the tower is 35.2 ℃, and the temperature of a kettle of the tower is 35.3 ℃. After washing, 5kg of the replacement water was discharged to the water tank V2, and 5.2kg of water was added.
(5) After hydrolysis, 90kg of hydrochloric acid with the concentration of 20wt% is injected into the hydrolysis kettle, stirred for 30min and then enters the standing tank through the filter.
(6) After standing for 2 hours, the oil-water interface was sufficiently layered. The oil phase is aqueous solvent and sent to the solvent recovery tower, the water phase is sent to the water tank for recycling, and 50kg of waste water is discharged in order to avoid salt separation.
(7) The theoretical plate number of the solvent recovery tower is 10, the operation pressure is 0.05MPag, the tower top temperature is 45.2 ℃, and the tower kettle temperature is 116.3 ℃. And (3) dehydrating the solvent collected at the tower top to 10ppm through a drying tower T3 to an alkyl aluminum dilution tank V1, and discharging residual liquid at the tower bottom.
The composition of the content of each stream in fig. 1 in this example 1 is shown in table 2 below.
Table 2:
[ example 2 ] A method for producing a polycarbonate
The alkyl aluminum hazardous waste shown in the table 1 is treated by adopting the device shown in the figure 1.
V1 dilution tank; a V2 water tank; a V3 acid medium tank; v4 standing tank; v5 solvent recovery storage tank; t1, washing a tower with water; a T2 solvent recovery column; t3, a drying tower; r1 hydrolysis kettle; an SR1 filter; s1, aluminum alkyl hazardous waste; s2, inert organic solvent; s3, hydrolyzing and supplementing water; s4, an acidic medium; s5, washing with water to supplement water; s6, oil phase; s7, waste water; s8, waste gas; s9, waste liquor; s10, replacing water.
(1) 50kg of toluene was placed in a dilution tank, and the alkylaluminum hazardous wastes were injected at a rate of 30kg/min and mixed by nitrogen blowing while cooling by circulating water through a jacket, the maximum temperature in the tank was not higher than 35 ℃ and the trimethylaluminum content in the alkylaluminum dilute solution was 7.67% by weight.
(2) 1000kg of water is introduced into the hydrolysis kettle, stirring is started, and circulating water is introduced into a jacket. The dilute solution of aluminum alkyl is injected into the hydrolysis kettle at the speed of 15 kg/min.
(3) The hydrolysis process was continued for 30min with stirring and cooling, the maximum temperature of the hydrolysis kettle was 41.7 ℃.
(4) The gas phase product obtained in the hydrolysis process enters a water washing tower for water washing treatment and then is discharged out of a boundary area, the number of theoretical plates of the water washing tower is 4, the operation pressure is 0.07MPag, the temperature of the top of the tower is 35.8 ℃, and the temperature of the bottom of the tower is 36.6 ℃. After washing, 5kg of the replacement water was discharged to the water tank V2, and 5.2kg of water was added.
(5) After the hydrolysis, 90kg of hydrochloric acid with the concentration of 20wt% is injected into the hydrolysis kettle, stirred for 30min and then enters the standing tank through the filter.
(6) After standing for 2 hours, the oil-water interface was sufficiently layered. The oil phase is aqueous solvent and sent to the solvent recovery tower, the water phase is sent to the water tank for recycling, and 50kg of waste water is discharged in order to avoid salt separation.
(7) The number of theoretical plates of the solvent recovery tower is 8, the operating pressure is 0.04MPag, the temperature at the top of the tower is 44.6 ℃, and the temperature at the bottom of the tower is 121.9 ℃. And (3) dehydrating the solvent collected at the tower top to 20ppm through a drying tower T3 to an alkyl aluminum dilution tank V1, and discharging residual liquid at the tower bottom.
The composition of the content of each stream in fig. 1 in this example 2 is shown in table 3 below.
Table 3:
comparative example 1
The procedure of example 1 was repeated except that: the hydrolysis treatment was not followed by the acid hydrolysis treatment, and the other conditions were not changed.
After standing, the water content of the oil phase obtained by the standing tank is increased to 4.6w%, and after separation by the solvent recovery tower, the waste liquid is increased to 76kg, so that the solvent recovery effect is obviously reduced. The water content of the recovered solvent is higher, and the water content of the recovered solvent is 392ppm after the same condition is passed through the drying tower.
The content composition of each stream (not containing stream S4) in fig. 1 in this comparative example 1 is shown in table 4 below.
Table 4:
comparative example 2
The procedure of example 1 was repeated except that: the dilute solution of aluminum alkyl is injected into the hydrolysis kettle at a speed of 260 kg/min.
Under the action of stirring and cooling, the hydrolysis process lasts for 20min, the maximum temperature of the hydrolysis kettle is 66.2 ℃, and the local overheating temperature is higher.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (13)
1. A method for treating aluminum alkyl hazardous waste comprises the following steps:
(1) Diluting the aluminum alkyl hazardous waste by using an inert organic solvent to obtain a diluent; the inert organic solvent is selected from organic solvents which do not react with water;
(2) Injecting the diluent into water, stirring and hydrolyzing to obtain hydrolysate; in the step (2), the injection amount per minute is not more than 15% of the total weight of the diluent;
(3) Adding an acidic medium into the hydrolysate, wherein the acidic medium is at least one of hydrochloric acid, nitric acid and sulfuric acid, and stirring for acidolysis treatment to obtain a mixed solution.
2. The process according to claim 1, characterized in that, in step (1),
the inert organic solvent is at least one selected from toluene, hexane, petroleum ether, benzene and octane; and/or
In the diluent in the step (1), the weight content of the aluminum alkyl hazardous waste is less than 10wt%; and/or
The dilution in step (1) is carried out at a temperature below 45 ℃.
3. The process according to claim 2, characterized in that in the dilution of step (1) the content by weight of the alkylaluminium hazardous wastes is less than 5% by weight.
4. The processing method according to claim 1,
in the step (1), the alkyl aluminum hazardous waste is injected into the inert organic solvent; the injection amount per minute is not higher than 40% of the total amount of the alkyl aluminum hazardous waste; and/or
In step (2), the injection amount per minute is not more than 10% of the total weight of the diluent.
5. The processing method according to claim 4,
in the step (1), the alkyl aluminum hazardous waste is injected into the inert organic solvent, and the injection amount per minute is not more than 30% of the total amount of the alkyl aluminum hazardous waste.
6. The processing method according to claim 1,
in the step (2), the weight ratio of the total amount of water to the diluent obtained in the step (1) is more than or equal to 1:3; and/or
The hydrolysis in the step (2) is carried out at a temperature below 45 ℃; and/or
And (3) performing hydrolysis in the step (2) in a container with a stirring function and a cooling function, or performing hydrolysis in a container with a nitrogen blowing function and a cooling function.
7. The treatment method according to claim 1, wherein a gas-phase product is generated in the hydrolysis process in the step (2), and the gas-phase product is introduced into a water washing tower to be subjected to water washing treatment.
8. The process according to claim 7, wherein the number of theoretical plates of the water washing column is 1 to 5, the operating pressure is 0.01 to 0.60MPag, the temperature at the top of the column is 25 to 45 ℃ and the temperature at the bottom of the column is 35 to 46 ℃.
9. The process of claim 1, wherein, in step (3),
the molar ratio of the hydrogen ions in the acidic medium to the aluminum alkyl is (1-10): 1.
10. The process of claim 9, wherein, in step (3),
the molar ratio of the hydrogen ions to the aluminum alkyl in the acidic medium is (2-6): 1.
11. The process according to one of claims 1 to 10, characterized in that step (3) is followed by steps (4) and (5):
(4) Filtering and standing the mixed solution to obtain an oil phase and a water phase;
(5) And (3) recovering the solvent from the obtained oil phase, discharging a part of the obtained water phase, and recycling the rest water phase as the hydrolysis water in the step (2).
12. The process of claim 11, wherein the solvent recovery in step (5) is carried out in a solvent recovery tower, the oil-containing water phase in the bottom of the tower is discharged from the battery limit, and the oil phase obtained at the top of the tower is recycled as the diluent in step (1).
13. The process of claim 12, wherein the theoretical plate number of the solvent recovery column is 5 to 20, the operating pressure is 0.01 to 0.60MPag, the overhead temperature is 25 to 100 ℃, and the kettle temperature is 45 to 250 ℃.
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| GB808055A (en) * | 1956-04-18 | 1959-01-28 | Exxon Research Engineering Co | Aluminium trialkyls and alcohols prepared therefrom |
| CN103182156B (en) * | 2011-12-28 | 2016-04-06 | 中国石油天然气股份有限公司 | Recovery processing method of dangerous waste in alkyl aluminum production process |
| CN102961844A (en) * | 2012-11-28 | 2013-03-13 | 大连东泰产业废弃物处理有限公司 | Harmless treatment method of waste triethyl aluminum |
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