CN112791561B - Trimethyl phosphite rectification tail gas deodorization method and equipment - Google Patents

Trimethyl phosphite rectification tail gas deodorization method and equipment Download PDF

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CN112791561B
CN112791561B CN202110042034.7A CN202110042034A CN112791561B CN 112791561 B CN112791561 B CN 112791561B CN 202110042034 A CN202110042034 A CN 202110042034A CN 112791561 B CN112791561 B CN 112791561B
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trimethyl phosphite
tail gas
purification
adsorbent
layer
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CN112791561A (en
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蒋飚
郭之军
李能武
赵和英
张光祥
彭小敏
王雲
倪嘉怡
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Guizhou Wylton Jinglin Electronic Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1487Removing organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1431Pretreatment by other processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1431Pretreatment by other processes
    • B01D53/1437Pretreatment by adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1493Selection of liquid materials for use as absorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18Absorbing units; Liquid distributors therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81Solid phase processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/10Oxidants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/10Oxidants
    • B01D2251/106Peroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20Organic absorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20Organic absorbents
    • B01D2252/202Alcohols or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20Organic absorbents
    • B01D2252/202Alcohols or their derivatives
    • B01D2252/2021Methanol
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2252/00Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20Organic absorbents
    • B01D2252/205Other organic compounds not covered by B01D2252/00 - B01D2252/20494
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20Organic adsorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20Organic adsorbents
    • B01D2253/204Metal organic frameworks (MOF's)

Abstract

The application discloses a trimethyl phosphite rectification tail gas deodorization method and equipment, and the method comprises the following steps: carrying out first purification on trimethyl phosphite tail gas generated under the rectification working condition; and carrying out second purification on the gas output after the first purification. Through this application solve the tail gas stench problem that the trimethyl phosphite rectification among the prior art produced, reduced the stench in the tail gas that the trimethyl phosphite rectification produced to a certain extent, be favorable to environmental protection and staff's physical and mental health.

Description

Trimethyl phosphite rectification tail gas deodorization method and equipment
Technical Field
The application relates to the field of waste gas treatment in chemical production, in particular to a trimethyl phosphite rectification tail gas deodorization method and equipment.
Background
Among semiconductor deposition materials, trimethyl phosphite (TMP) is the main phosphorus source for deposition of phosphosilicate glass (PSG) and borophosphosilicate glass (BPSG) during wafer fabrication. However, when phosphosilicate glass (PSG) and borophosphosilicate glass (BPSG) are produced, TMP is required to be rectified only when the main content of TMP is more than 99.99% and the purity of TMP is more than 8.5N.
The inventor finds that the process is simple to use, but the TMP is volatile, so that pungent bitter odor is generated, the on-site malodor is easily caused, the body health of production personnel is damaged, and the normal operation of production operation is not facilitated. In most of the prior patents, for example, in the CN107840858A trimethyl phosphite continuous vacuum rectification process, no key description is made on tail gas treatment, only tail gas is sent to a tail gas treatment tower, and the tail gas treatment and purification effect is not specifically described; patents CN101306900A, CN105314780A, etc. also only aim at the wastewater treatment process of TMP, and do not mention how to treat the field odor caused by volatilization of trimethyl phosphite; in the control of trimethyl phosphite odor in the second stage 1997 in Henan chemical industry, a process and equipment for treating tail gas are provided, a water absorption tower and a chemical oxidation tower are used for treating the tail gas, and then the tail gas is discharged. Therefore, the problem of the foul smell of the tail gas generated by the rectification of trimethyl phosphite is not taken into consideration and well solved.
Disclosure of Invention
The application provides a method and equipment for deodorizing trimethyl phosphite rectification tail gas, which are used for solving the problem of tail gas malodor generated by trimethyl phosphite rectification in the prior art.
According to one aspect of the application, a trimethyl phosphite rectification tail gas deodorization method is provided, and comprises the following steps: carrying out first purification on trimethyl phosphite tail gas generated under the rectification working condition; carrying out second purification on the gas output after the first purification; wherein the first purge uses an organic solvent and the second purge uses at least one of an oxidant and an adsorbent; alternatively, the first purge uses at least one of the oxidant and the adsorbent, and the second purge uses the organic solvent; the organic solvent is at least used for dissolving trimethyl phosphite in the tail gas, the adsorbent is used for adsorbing trimethyl phosphite in the tail gas, and the oxidant is used for oxidizing trimethyl phosphite in the tail gas.
Further, the organic solvent is used for dissolving trimethyl phosphite, boron trichloride and triethylamine in the tail gas.
Further, the dissolving capacity of trimethyl phosphite of the organic solvent is 15g-50g/100g, and the dissolving capacity of other gases is 10g-60g/100 g.
Further, the organic solvent is methanol, ethanol, ether, benzene, acetone, carbon tetrachloride and other solvents; the organic solvent is preferably ethanol.
Further, the adsorbent comprises: ester adsorbents, MOFs, or adsorption resins; and/or, the oxidizing agent comprises: activated alumina, manganese dioxide, potassium permanganate, sodium peroxide Na2O2, potassium peroxide K2O2, magnesium peroxide MgO2 or calcium peroxide CaO 2. Preferably 3 kinds of activated alumina, potassium permanganate and sodium peroxide are matched for use or 3 kinds of sodium peroxide, potassium peroxide and calcium peroxide are matched for use.
According to another aspect of the present application, there is also provided trimethyl phosphite rectification tail gas deodorization equipment for performing the above method, the equipment comprising: a first purification device for performing the first purification; a second purification device connected to the first purification device for performing the second purification.
Further, the bottom of the second purification device is connected with the first purification device, and the upper end of the second purification device is used for exhausting; the second purification device comprises at least two layers of sieve plates, and the oxidant and the adsorbent are respectively placed on the two layers of sieve plates.
Further, the gas passes through a first sieve plate and a second sieve plate in the two layers of sieve plates from the bottom of the second purification device in sequence, wherein the first sieve plate is arranged between the bottom of the second purification device and the second sieve plate, the oxidant is placed between the first sieve plate and the second sieve plate, and the adsorbent is placed between the second sieve plate and the upper end of the second purification device.
Further, a first number of movable filter screen cylinders for containing the oxidant are arranged above the first sieve plate, and a second number of movable filter screen cylinders for containing the adsorbent are arranged above the second sieve plate.
Furthermore, the second sieve tray in the second purifying device tank is movable, so that the filter screen barrel above the first sieve tray can be conveniently taken down, and the first and second filter screen barrels in the first layer can be omitted when the amount of the trimethyl phosphite tail gas is 1-100L.
Further, when the continuous rectification or the trimethyl phosphite tail gas treatment amount exceeds about 100L, the second sieve plate can be taken down and put into the first and second filter screen barrels, and the third, fourth, fifth and sixth filter screen barrels are also put above the second sieve plate.
Further, it is convenient to set up portable filter screen bucket firstly for changing oxidant and adsorbent, secondly can increase the quantity of oxidant and adsorbent according to the volume of handling trimethyl phosphite tail gas, and thirdly avoids filling too thick oxidant and adsorbent on first orifice plate and the second orifice plate, and the tail gas resistance of trimethyl phosphite increases, leads to the rectification operating mode to take place the accident.
Further, the oxidant and the adsorbent are placed in a filter bag.
The method comprises the following steps: carrying out first purification on trimethyl phosphite tail gas generated under the rectification working condition; carrying out second purification on the gas output after the first purification; wherein the first purge uses an organic solvent and the second purge uses at least one of an oxidant and an adsorbent; alternatively, the first purge uses at least one of the oxidant and the adsorbent, and the second purge uses the organic solvent; the organic solvent is at least used for dissolving trimethyl phosphite in the tail gas, the adsorbent is used for adsorbing trimethyl phosphite in the tail gas, and the oxidant is used for oxidizing trimethyl phosphite in the tail gas. Through this application solve the tail gas stench problem that the trimethyl phosphite rectification among the prior art produced, reduced the stench in the tail gas that the trimethyl phosphite rectification produced to a certain extent, be favorable to environmental protection and staff's physical and mental health.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, are included to provide a further understanding of the application, and the description of the exemplary embodiments of the application are intended to be illustrative of the application and are not intended to limit the application. In the drawings:
FIG. 1 is a flow chart of a method for deodorizing trimethyl phosphite rectification tail gas according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a trimethyl phosphite rectification tail gas deodorization device according to an embodiment of the invention.
The reference numbers are as follows:
10. a first purification device; 11. a first air inlet; 12. a first exhaust port; 13. a first liquid injection port; 14. a first drain port; 20. a second purification device; 21. a second air inlet; 22. a second exhaust port; 40. a first perforated screen; 41. a first screen drum; 42. a second screen drum; 50. a second perforated deck; 51. a third screen drum; 52. a fourth screen drum; 53. a fifth screen drum; 54. a sixth screen drum; 30. filling an oxidant filter bag 1; 31. filling an oxidant filter bag 2; 32. filling an oxidant filter bag 3; 60. filling the adsorbent filter bag 1; 61. filling the adsorbent filter bag 2; 62. filling the adsorbent filter bag 3; 63. filling the adsorbent filter bag 4; 64. filling the adsorbent filter bag 5; 70. and (4) an exhaust pipeline.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in the process, method, article, or apparatus that comprises the element.
In this embodiment, a method for deodorizing trimethyl phosphite rectification tail gas is provided, and fig. 1 is a flow chart of the method for deodorizing trimethyl phosphite rectification tail gas according to the embodiment of the present invention, as shown in fig. 1, the method includes the following steps:
step S102, carrying out first purification on trimethyl phosphite tail gas generated under the rectification working condition;
step S104, carrying out second purification on the gas output after the first purification; wherein the first purge uses an organic solvent and the second purge uses at least one of an oxidant and an adsorbent; alternatively, the first purge uses at least one of the oxidant and the adsorbent, and the second purge uses the organic solvent; the organic solvent is at least used for dissolving trimethyl phosphite in the tail gas, the adsorbent is used for adsorbing trimethyl phosphite in the tail gas, and the oxidant is used for oxidizing trimethyl phosphite in the tail gas.
Through the steps, purification is carried out twice, and different modes are used for purification each time, so that tail gas can be effectively purified and deodorized.
In this embodiment, the organic solvent is methanol, ethanol, diethyl ether, benzene, acetone, carbon tetrachloride, or the like; the organic solvent is preferably ethanol.
In this embodiment, the adsorbent comprises: ester adsorbents, MOFs, or adsorption resins; and/or, the oxidizing agent comprises: activated alumina, manganese dioxide, potassium permanganate, sodium peroxide Na2O2, potassium peroxide K2O2, magnesium peroxide MgO2 or calcium peroxide CaO 2. Preferably 3 kinds of activated alumina, potassium permanganate and sodium peroxide are matched for use or 3 kinds of sodium peroxide, potassium peroxide and calcium peroxide are matched for use.
As an added embodiment, the trimethyl phosphite tail gas after the first purification and the second purification is analyzed, when trimethyl phosphite in the tail gas exceeds a first threshold value, the tail gas after the first purification and the second purification is subjected to the first purification and the second purification, the tail gas is continuously collected, and when the number of times that trimethyl phosphite in the purified tail gas exceeds the first threshold value reaches a preset value within a preset time period, first warning information is sent, wherein the first warning information is used for prompting the replacement of the organic solvent, the adsorbent and the oxidant.
After a new replacement of the organic solvent, the flow rate and flow rate of the gas subjected to the first purification are recorded before the first purification is performed, and the change in the content of trimethyl phosphite in the gas subjected to the first purification is detected between the first purification and the second purification, establishing a relationship between the amount of organic solvent, the amount of purified gas and other amounts that can also be purified. And after the new organic solvent is replaced every time, calculating the amount of gas which can be purified, and when the amount of the gas which can be purified is lower than a second threshold value, sending second alarm information, wherein the second alarm information is used for prompting the replacement of the organic solvent.
After receiving the first warning message, judging whether a second warning message is received within a preset time period before receiving the first warning message, if the second warning message is received, replacing the organic solvent, and if the second warning message is not received, replacing the adsorbent and the oxidant.
In order to implement the method, in this embodiment, there is also provided a trimethyl phosphite rectification tail gas deodorization device, which is used for executing the method, and includes: a first purification device for performing the first purification; a second purification device connected to the first purification device for performing the second purification.
In this embodiment, there is provided a preferable structure of the purification apparatus, wherein the bottom of the second purification apparatus is connected to the first purification apparatus, and the upper end of the second purification apparatus is used for exhaust gas; the second purification device comprises at least two layers of sieve plates, and the oxidant and the adsorbent are respectively placed on the two layers of sieve plates.
In a preferable structure, the gas passes through a first sieve plate and a second sieve plate in the two sieve plates from the bottom of the second purification device in sequence, wherein the first sieve plate is arranged between the bottom of the second purification device and the second sieve plate, the oxidant is arranged between the first sieve plate and the second sieve plate, and the adsorbent is arranged between the second sieve plate and the upper end of the second purification device.
In order to facilitate replacement of the adsorbent or the oxidant, a first number of movable filter screen cylinders for placing the oxidant are arranged on the first sieve plate, and a second number of movable filter screen cylinders for placing the adsorbent are arranged on the second sieve plate. More preferably, the oxidant and the adsorbent may be placed in a filter bag.
The method and the equipment for deodorizing trimethyl phosphite (TMP) rectification tail gas provided by the embodiment and the preferred embodiment have the advantages of simple process flow, simple purification equipment, small occupied area and good treatment effect. Mainly used for solving the problem of site malodor caused by tail gas, and the malodor is mainly from trimethyl phosphite.
This is described below in connection with a preferred embodiment.
In this embodiment, the apparatus (or referred to as a device) shown in fig. 2 is used, and as shown in fig. 2, the apparatus includes: the device comprises a first purification device 10, a first air inlet 11, a first exhaust port 12, a first liquid injection port 13, a first liquid exhaust port 14, a second purification device 20, a second air inlet 21, a second exhaust port 22, a first sieve plate 40, a first filter screen barrel 41, a second filter screen barrel 42, a second sieve plate 50, a third filter screen barrel 51, a fourth filter screen barrel 52, a fifth filter screen barrel 53, a sixth filter screen barrel 54, filling oxidant filter bags 1-30, filling oxidant filter bags 2-31, filling oxidant filter bags 3-32, filling adsorbent filter bags 1-60, filling adsorbent filter bags 2-61, filling adsorbent filter bags 3-62, filling adsorbent filter bags 4-63, filling adsorbent filter bags 5-64 and a tail gas pipeline 70.
The method for treating the exhaust gas in the present embodiment will be described with reference to the above-mentioned apparatuses.
(1) Under the normal rectification working condition, the generated trimethyl phosphite tail gas enters a first purification device through the pipeline control input, and an organic solvent capable of dissolving trimethyl phosphite is added into the first purification device. The dissolving capacity of trimethyl phosphite is 15-50g/100g solvent. The solvent includes organic solvents such as methanol, ethanol, diethyl ether, benzene, acetone, carbon tetrachloride, etc. Ethanol should preferably be used as solvent.
The solvent is added from the first liquid injection port, the adding amount is determined according to the treatment amount of the rectification tail gas, and 10-60L is generally preferred.
(2) More than half trimethyl phosphite tail gas that comes out from first purifier gets into second purifier, and gaseous getting into from the second purifier bottom, upper end exhaust, second purifier are a jar body of double-deck sieve mesh plate structure, and two-layer about jar body divides, and the below is first layer sieve mesh plate, and first layer sieve mesh plate top sets up two portable filter screen cylinders. Jar body top is the portable sieve mesh of second floor, and second floor sieve mesh top sets up four portable filtration screen drums, sets up portable filtration screen drum and second floor sieve mesh firstly for convenient change oxidant and adsorbent, secondly considers the decision of handling the tail gas volume to increase oxidant and adsorbent quantity. The first layer of sieve plate is provided with an oxidant filled by a filter bag, and the first and second filter screen cylinders are internally provided with the oxidant filled by the filter bag; similarly, the second layer of sieve plate is provided with the adsorbent filled by the filter bag, and the third to sixth filter screen cylinders are also filled with the adsorbent by the filter bag. Therefore, the lower half part of the tank body is a tail gas reaction layer, and oxidants are needed, wherein the oxidants include conventional oxidants such as active aluminum oxide, manganese dioxide, potassium permanganate, sodium peroxide Na2O2, potassium peroxide K2O2, magnesium peroxide MgO2, calcium peroxide CaO2 and the like. Preferentially using 3 kinds of activated alumina, potassium permanganate and sodium peroxide in a matching way or 3 kinds of sodium peroxide, potassium peroxide and calcium peroxide in a matching way, reacting trimethyl phosphite with an oxidant to generate trimethyl phosphate, wherein the reaction is carried out at normal temperature and normal pressure, and the reaction formula is as follows:
Figure BDA0002896279590000061
the use requirement of the filter bag is explained, the material of the filter bag can be polyacrylonitrile, polytetrafluoroethylene and other base materials with better acid and alkali resistance, the breaking strength is 500-2000N/cm, the breaking elongation is 10-60%, the air permeability is 10-60m 3/square meter/min, and the use temperature is less than or equal to 130 ℃.
The second layer of sieve plate is provided with an adsorbent filled by filter bags, and the four filter screen cylinders are filled with the filter bags filled with the adsorbent. One or more adsorbents can be used in combination, and the adsorbents comprise ester adsorbents, MOFs (metal-organic frameworks) or adsorption resins. The adsorbent has good absorption effect on ester substances, high absorption rate, high capacity and excellent diffusion performance, and can adsorb and enrich ester organic substances, thereby achieving the purpose of absorbing residual trimethyl phosphite in tail gas.
In the embodiment, two purification devices, namely a first purification device and a second purification device, are adopted, wherein the first purification device is added with a solvent capable of dissolving trimethyl phosphite, such as ethanol or industrial ethanol; the air inlet pipe is introduced into the solvent, and the upper end of the air inlet pipe is used for exhausting air; the second purifying device is a two-layer structure, and the filter bag filled with the oxidant, such as active aluminum oxide, manganese dioxide, potassium permanganate, sodium peroxide, potassium chlorate, ferric chloride and other conventional oxidants, are placed in the first layer of sieve plate and the filter screen cylinder. The second layer of sieve plate and the filter screen cylinder are provided with filter bags filled with adsorbents, and the adsorbents comprise ester adsorbents, MOFs or adsorption resin and the like.
In this embodiment, the trimethyl phosphite tail gas is transported to a first purification device through a pipeline, and the first purification device is filled with ethanol solvent to dissolve trimethyl phosphite in the tail gas. After the dissolution treatment, the residual trimethyl phosphite gas which is not dissolved and absorbed is conveyed to a second purification device, and firstly enters a first layer of the second purification device, and trimethyl phosphite reacts with an oxidant of the first layer and then enters a second layer of the second purification device. And after the gas passes through the second layer of the second purifying device and is fully contacted with the ester adsorbent, the unreacted trimethyl phosphite gas is adsorbed.
After the treatment process is adopted, GB/T14675-93 'determination of air quality and odor, three-point comparison type odor bag method' is used for determining the treatment effect before and after deodorization, wherein the odor concentration before deodorization is 354813 (dimensionless) and the odor concentration after deodorization is 57.5 (dimensionless). The results of odor concentration measurement before and after deodorization are shown in tables I and II. After deodorization, the odor concentration reaches the secondary standard of the factory boundary of GB14554-93 discharge Standard of malodorous pollutants.
TABLE-measurement of trimethyl phosphite Tail gas before deodorization
Figure BDA0002896279590000071
Note: 0 is the correct answer and X is the wrong answer.
Results of measurement of deodorized trimethyl phosphite tail gas
Figure BDA0002896279590000072
Note: 0 is the correct answer and X is the wrong answer.
The method and the device for deodorizing trimethyl phosphite rectification tail gas have the following advantages: 1. the process is simple and feasible, safe, efficient, simple and convenient to operate, simple in structure of the purification device, low in material and equipment cost, small in occupied area and good in treatment effect, and the exhausted tail gas can reach the first-level to second-level emission standard of a factory boundary; 2. the whole trimethyl phosphite rectification tail gas is in a closed environment, so that stink caused by leakage can not be caused, the harm to the body of field operators is greatly reduced, and green and environment-friendly production is really realized.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims (7)

1. A trimethyl phosphite rectification tail gas deodorization method is characterized by comprising the following steps:
carrying out first purification on trimethyl phosphite tail gas generated under the rectification working condition;
carrying out second purification on the gas output after the first purification;
wherein the first purge uses an organic solvent and the second purge uses an oxidant and an adsorbent; the organic solvent is at least used for dissolving trimethyl phosphite in the tail gas, the adsorbent is used for adsorbing trimethyl phosphite in the tail gas, and the oxidant is used for oxidizing trimethyl phosphite in the tail gas; the adsorbent comprises: ester adsorbents, MOFs, or adsorption resins;
the trimethyl phosphite tail gas is conveyed to a first purifying device through a pipeline for first purification, the nonabsorbed trimethyl phosphite gas passing through the first purifying device enters a second purifying device, the bottom of the second purifying device is connected with the first purifying device, the upper end of the second purifying device is used for exhausting, the second purifying device is a tank body of a double-layer sieve pore plate structure, the tank body is divided into an upper layer and a lower layer, a first layer of sieve pore plate is arranged below the tank body, and two movable filter screen cylinders are arranged above the first layer of sieve pore plate; a second layer of movable sieve plate is arranged above the tank body, four movable filter screen cylinders are arranged above the second layer of sieve plate, and an oxidant filled by a filter bag is placed in the filter screen cylinder on the first layer of sieve plate; the filter screen cylinder on the second layer of sieve plate is filled with the adsorbent by the filter bag.
2. The method of claim 1, wherein the organic solvent is used to dissolve trimethyl phosphite, boron trichloride, and triethylamine in the tail gas.
3. The method according to claim 2, wherein the organic solvent has a dissolving power of trimethyl phosphite of 15g to 50g/100g, and the other gas has a dissolving power of 10g to 60g/100 g.
4. The method of claim 3, wherein the organic solvent is methanol, ethanol, diethyl ether, benzene, acetone, or carbon tetrachloride.
5. The method according to any one of claims 1 to 4,
the oxidizing agent comprises: activated alumina, manganese dioxide, potassium permanganate, sodium peroxide Na2O2, potassium peroxide K2O2, magnesium peroxide MgO2 or calcium peroxide CaO 2.
6. The method according to claim 5, wherein 3 kinds of activated alumina, potassium permanganate and sodium peroxide are used in combination as the oxidizing agent or 3 kinds of sodium peroxide, potassium peroxide and calcium peroxide are used in combination as the oxidizing agent.
7. A trimethyl phosphite rectification tail gas deodorization device for performing the method of any one of claims 1 to 6, the device comprising: the first purification device and the second purification device.
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