Continuous deep dehydration device for anisole for boron isotope separation

Abstract

The invention provides a continuous deep dehydration device for anisole for boron isotope separation, which comprises a silica gel primary dehydration drying tower and a molecular sieve deep dehydration drying tower which are sequentially connected in series, and the anisole is sequentially subjected to two-step dehydration treatment, firstly, the anisole subjected to silica gel primary dehydration is limited to meet the conditions that the purity is greater than or equal to 99.5 wt% and the water content is 80-120ppm, and then the anisole subjected to molecular sieve deep dehydration is subjected to secondary dehydration treatment; the method comprises the following steps: carrying out silica gel primary dehydration on anisole to make water in the anisole preliminarily adsorbed by silica gel particles, carrying out molecular sieve deep dehydration on the anisole containing trace water to make the trace water be further fully dehydrated by a molecular sieve so as to obtain anisole for boron isotope separation and make the water content be less than or equal to 10 ppm, and carrying out silica gel primary dehydration on the anisole containing trace water to make the anisole containing trace water be less than or equal to 10 ppm. The continuous deep dehydration device is simple in structure and high in safety, the production cost can be further reduced by means of regeneration of silica gel particles and molecular sieve particles, and industrial application and popularization are facilitated.

Description

Technical Field

[0001] The invention relates to the technical field of boron isotope separation, in particular to a complexing agent anisole used for boron isotope separation, and in particular to a continuous deep dehydration device of anisole used for boron isotope separation. Background Art

[0002] Stable isotope boron-10 ( 10 B) Due to its unique neutron absorption characteristics, it is increasingly used in modern nuclear industry, military equipment and medicine. 10 B products include boron-10 acid, boron-10 powder, boron carbide, boron nitride and other products with different abundance requirements. The industrial chain is long and the product application fields are wide, especially playing an important role in alleviating the global petrochemical energy shortage. The application of such products in the nuclear energy field makes it possible to widely develop and apply economic, safe and clean nuclear energy resources.

[0003] Since the isotope boron-10 has a much larger thermal neutron capture area than boron-11, it is widely used in the nuclear industry to manufacture thermal neutron counters, reactor control rods and thermal neutron shielding materials, especially in boron neutron cancer treatment methods (BNCT). The abundance of boron-10 in nature is only 19-20%, so it is necessary to enrich and purify the boron-10 isotope.

[0004] The chemical exchange distillation method of boron trifluoride anisole is a process technology first invented in the United States. It started in the mid-1970s and reached full production in 1977 with a production scale of 2 tons / year, and the boron-10 abundance can reach 92%. This process technology has advantages because it operates under normal temperature and pressure conditions and has a higher separation coefficient. Although the process of preparing anisole complex from raw materials is slightly longer than that of methyl and ethyl ether complex materials, its basic material anisole is recycled in the whole process of the production system, and the final product is enriched boron trifluoride-10 ( 10 BF3) and boron trifluoride-11( 11 BF3), both of which are high value-added terminal technology products. In terms of cost and benefit accounting, they have obvious advantages over the methyl and ethyl ether methods, making the production cost much lower. Currently, the United States and Georgia both use this process technology route.

[0005] Anisole is widely used in the fields of drug synthesis, dye synthesis, spice blending as an important raw material, intermediate and solvent. The water content of anisole of technical grade is relatively low, generally at several hundred ppm, or even lower. However, when anisole is used for the chemical exchange rectification method of boron trifluoride anisole to realize boron isotope separation, further dehydration is required. As separated object, the raw material boron trifluoride gas of isotope boron-10 and isotope boron-11 is very easy to react with water, and the hydrofluoric acid produced has extremely strong corrosiveness, and violent heat release, and by-products are also easy to block pipelines, reduce heat exchange efficiency and conveying efficiency, therefore need anisole to carry out deep dehydration, it is generally believed that water content needs to be reduced to below 30ppm, even to below 10ppm, thereby ensuring production safety, extending equipment service life, reducing the generation of by-products, and improving production efficiency.

[0006] At present, commonly used anisole dehydration methods include physical adsorption method and chemical reaction method. The molecular sieve drying method in the physical adsorption method, such as the preparation method of a super dry organic solvent disclosed in CN 112479797 A, needs to be carried out in a glove box and in a nitrogen atmosphere, and the reaction conditions are harsh, and it is not suitable for industrialized continuous scale production. The water gas reaction method in the chemical reaction method, such as the boron isotope separation complexing agent anisole refining and purification method disclosed in CN 107573224 A, uses CO to react with the water in anisole under catalytic conditions to remove trace water, although the reaction has a large dehydration depth, it needs to be carried out under high temperature and high pressure conditions, not only additional reaction equipment is required, but also the reaction conditions are relatively harsh, in addition, the raw material used in the reaction system is CO and one of the products is H2, not only flammable and explosive, but also highly toxic, and has high requirements for the operating environment.

[0007] In summary, it is necessary to provide a simple continuous deep dehydration device for anisole suitable for boron isotope separation. Summary of the invention

[0008] In view of the problems existing in the prior art, the present invention provides a continuous deep dehydration device for anisole for boron isotope separation, comprising a silica gel primary dehydration drying tower and a molecular sieve deep dehydration drying tower which are sequentially connected in series, and anisole is sequentially subjected to two-step dehydration treatment to obtain anisole for boron isotope separation with a water content of ≤10ppm. The continuous deep dehydration device of the present invention has a simple structure and high safety, and can further reduce production costs by means of the regeneration of silica gel particles and molecular sieve particles, so as to facilitate industrial promotion and use.

[0009] To achieve this object, the present invention adopts the following technical solutions:

[0010] The object of the present invention is to provide a continuous deep dehydration device for anisole for boron isotope separation, the continuous deep dehydration device comprising a silica gel primary dehydration drying tower and a molecular sieve deep dehydration drying tower connected in series in sequence;

[0011] The silica gel primary dehydration drying tower is filled with silica gel particles, an inlet for primary dehydration anisole is provided at the top for adding anisole with a purity of ≥99.5wt% and a water content of 80-120ppm, an outlet for primary dehydration anisole is provided at the bottom, and an online moisture detector is provided at the outlet of the primary dehydration anisole for online monitoring of the water content of anisole discharged from the outlet of the primary dehydration anisole, so that anisole with a water content of ≤50ppm enters the molecular sieve deep dehydration drying tower;

[0012] The molecular sieve deep water removal drying tower is filled with molecular sieve particles, a deep water removal anisole inlet is arranged at the top and connected to the primary water removal anisole outlet, and a deep water removal anisole outlet is arranged at the bottom for discharging anisole with a water content of ≤10ppm for boron isotope separation.

[0013] The continuous deep dehydration device of the present invention sequentially performs two-step dehydration treatment of silica gel primary dehydration and molecular sieve deep dehydration, firstly limits the anisole for silica gel primary dehydration to meet the conditions of purity ≥99.5wt% and water content of 80-120ppm, then performs silica gel primary dehydration, so that the water in the anisole is preliminarily adsorbed by silica gel particles, the water content of the anisole obtained by silica gel primary dehydration is ≤50ppm, then the anisole containing trace water is subjected to molecular sieve deep dehydration, so that the trace water is further fully dehydrated by the molecular sieve, thereby obtaining anisole for boron isotope separation and the water content is ≤10ppm. The continuous deep dehydration device of the present invention has simple structure and high safety, and can also further reduce production costs by means of the regeneration of silica gel particles and molecular sieve particles, so as to be convenient for industrial popularization and use.

[0014] As a preferred technical solution of the present invention, a distillation tower is arranged in series upstream of the silica gel primary water removal drying tower to distill industrial anisole to obtain anisole with a purity of ≥99.5wt% and a water content of 80-120ppm.

[0015] As a preferred technical solution of the present invention, the distillation tower is a packed tower, the packed tower is provided with two sections of packing and feeding is carried out between the towers, and the packed tower adopts φ6×6θ mesh ring packing.

[0016] As a preferred technical solution of the present invention, the distillation tower is equipped with a temperature sensor and a pressure sensor.

[0017] As a preferred technical solution of the present invention, the diameter of the distillation tower is 80-120 mm, for example, 80 mm, 85 mm, 90 mm, 95 mm, 100 mm, 105 mm, 110 mm, 115 mm or 120 mm.

[0018] In the present invention, rectifying tower is used for initial dehydration, and rectifying tower is equipped with temperature and pressure sensor, and temperature is controlled at about the boiling point of anisole, and pressure is controlled at 120~140Pa / m, and tower still volume is as the criterion for meeting liquid holding demand, and tower diameter is 80~120mm, and two sections of packing towers are fed, and φ 6 × 6θ mesh ring filler is used, and the position connected with air must be equipped with nitrogen protection system (nitrogen bottle with pressure), and vacuumizing and nitrogen filling operation is alternated 3 times, and air and moisture in tower are excluded, and pressure in tower is kept to be slightly higher than atmospheric pressure, and water in air is prevented from entering system. In actual operation process, anisole is added in rectifying tower, and timing heating, after reaching the boiling point of anisole, total reflux 1 hour, stops heating, and discharge port collects material as fast as possible, and the first dehydration drying tower of silica gel entering downstream is prepared to continue dehydration.

[0019] As a preferred technical solution of the present invention, a first anisole storage tank, a chemical drying tower and a second anisole storage tank are sequentially arranged in series downstream of the molecular sieve deep water removal drying tower;

[0020] The chemical drying tower is a fixed bed reactor, with a chemical drying anisole inlet at the top for introducing anisole from a first anisole storage tank; a CO gas inlet at the bottom for introducing CO gas required for a chemical reaction; a catalyst fixedly arranged in the middle for catalyzing a water gas reaction in the chemical drying tower; a chemical drying waste gas outlet at the top for discharging waste gas generated by the water gas reaction; and a chemical drying anisole outlet at the bottom for discharging anisole with a water content of 1 to 3 ppm for boron isotope separation, and storing the anisole in a second anisole storage tank.

[0021] It should be noted that whether to perform ultra-deep water removal on the anisole obtained by deep water removal with molecular sieve to further reduce the water content of anisole can be selected by those skilled in the art according to actual needs.

[0022] As a preferred technical solution of the present invention, the internal volume of the chemical drying tower is 100-200L, for example, 100L, 110L, 130L, 150L, ​​160L, 180L or 200L, and the ratio of height to diameter is 2-3, for example, 2, 2.1, 2.2, 2.4, 2.5, 2.7, 2.9 or 3, etc.

[0023] In the present invention, chemical drying tower is used for ultra-deep water removal, adopts fixed bed reactor, reactor body adopts stainless steel, bears high temperature and pressure and corrosion resistance, components such as internal agitator are adapted to main body material, mainly select corrosion-resistant material, ensure long-term stable operation. The anisole through two-step dehydration treatment is added into reactor, CO gas under operating pressure is passed, reacts with water in anisole, is heated to reaction temperature, reaction time is 3~5 hours, after reaction finishes, collects material by discharging port, enters sealed raw material storage tank, decompresses and removes reaction and generates gas mixture (CO, H2 and CO2).

[0024] As a preferred technical solution of the present invention, the silica gel primary water removal drying tower adopts a fixed bed with a bed height of 30 to 50 cm, such as 30 cm, 35 cm, 40 cm, 45 cm or 50 cm, and an inner diameter of 6 to 10 cm, such as 6 cm, 6.5 cm, 7 cm, 7.5 cm, 8 cm, 8.5 cm, 9 cm, 9.5 cm or 10 cm.

[0025] As a preferred technical solution of the present invention, the silica gel primary water removal drying tower is connected in parallel with a silica gel primary water removal standby tower, a switching valve is arranged on the upstream main pipeline of the two parallel connections, the online moisture detector is arranged on the downstream main pipeline of the two parallel connections, and the switching valve and the online moisture detector are respectively connected with the controller to realize electrical signal connection; once the online moisture detector monitors that the water content of anisole discharged from the primary water removal anisole outlet exceeds 50ppm, the controller controls the switching of the switching valve and uses the silica gel primary water removal standby tower to continue to realize continuous dehydration.

[0026] As a preferred technical solution of the present invention, the molecular sieve deep water removal drying tower adopts a fixed bed with a bed height of 30 to 50 cm, such as 30 cm, 35 cm, 40 cm, 45 cm or 50 cm, and an inner diameter of 10 to 15 cm, such as 10 cm, 11 cm, 12 cm, 13 cm, 14 cm or 15 cm.

[0027] A continuous deep dehydration method is carried out based on the aforementioned continuous deep dehydration device of anisole for boron isotope separation, and the continuous deep dehydration method comprises the following contents:

[0028] If the anisole to be dehydrated satisfies the requirements of purity ≥99.5wt% and water content of 80-120ppm, the product purity is high and no rectification treatment is required, and silica gel can be directly used for initial water removal; if the requirements of purity ≥99.5wt% and water content of 80-120ppm are not met, for example, industrial anisole with a purity of 94.5-95.5wt% and a water content of 0.8-1.2wt%, it is necessary to carry out rectification treatment, and the target temperature of rectification is controlled to be 150-155°C, and the target pressure of rectification is 120-140Pa / m, so that the anisole after rectification satisfies the requirements of purity ≥99.5wt% and water content of 80-120ppm;

[0029] Anisole with a purity of ≥99.5wt% and a water content of 80-120ppm is first subjected to silica gel initial dehydration, wherein the silica gel initial dehydration uses silica gel particles of 100-400 meshes, and the anisole flow rate of the silica gel initial dehydration is 50-100mL / min; the regeneration method of the silica gel particles comprises: drying at 130-150°C for 2-4h, and / or, drying by purging with dry nitrogen;

[0030] The anisole that has completed the initial dehydration of silica gel is subjected to deep dehydration by molecular sieve, wherein the deep dehydration by molecular sieve uses molecular sieve particles of 100 to 400 meshes, and the deep dehydration by molecular sieve uses molecular sieve particles of any one of models 4A, 5A or 13X, and the flow rate of the anisole for deep dehydration by molecular sieve is 50 to 100 mL / min; the regeneration method of the molecular sieve particles comprises: drying at 180 to 220° C. for 4 to 6 hours, and / or, drying by purging with dry nitrogen, to obtain anisole with a water content of ≤10 ppm;

[0031] If there is no strict requirement for further dehydration of the water content of anisole, the anisole with a water content of ≤10ppm obtained by deep dehydration of molecular sieve can be directly used for boron isotope separation; if there is a strict requirement for further dehydration of the water content of anisole, it is necessary to perform ultra-deep dehydration on the anisole with a water content of ≤10ppm obtained by deep dehydration of molecular sieve, mix the anisole obtained by deep dehydration of molecular sieve with CO gas, and perform ultra-deep dehydration under the action of a catalyst, the reaction pressure of the ultra-deep dehydration is 1.0-5.0MPa, the reaction temperature is 150-200°C, and the reaction time is 3-5h. The catalyst uses a copper-based catalyst to obtain anisole for boron isotope separation with a water content of 1-3ppm.

[0032] Compared with the prior art solutions, the present invention has at least the following beneficial effects:

[0033] (1) The continuous deep dehydration device of the present invention sequentially performs a two-step dehydration process of silica gel primary dehydration and molecular sieve deep dehydration, firstly limiting the anisole subjected to silica gel primary dehydration to meet the conditions of purity ≥99.5wt% and water content of 80-120ppm, then performing silica gel primary dehydration so that water in the anisole is preliminarily adsorbed by silica gel particles, and the water content of the anisole obtained by the silica gel primary dehydration is ≤50ppm, then performing molecular sieve deep dehydration on the anisole containing trace water so that the trace water is further fully dehydrated by the molecular sieve, thereby obtaining anisole for boron isotope separation with a water content of ≤10ppm;

[0034] (2) The continuous deep dehydration device of the present invention has a simple structure and high safety. It can also further reduce production costs by regenerating silica gel particles and molecular sieve particles, making it easier to promote and use in industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 is a schematic diagram of a continuous deep dehydration device for anisole used for boron isotope separation according to Example 1 of the present invention;

[0036] In the figure: 1-distillation tower; 2-silica gel primary water removal drying tower; 3-molecular sieve deep water removal drying tower; 4-first anisole storage tank; 5-chemical drying tower; 6-second anisole storage tank; 7-online moisture detector; 8-switching valve. DETAILED DESCRIPTION

[0037] The technical solution of the present invention is further described below with reference to the accompanying drawings and through specific implementation methods.

[0038] To better illustrate the present invention and facilitate understanding of the technical solution of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0039] Example 1

[0040] This embodiment provides a continuous deep dehydration device for anisole for boron isotope separation, such as Figure 1As shown, the continuous deep dehydration device comprises a rectifying tower 1, a silica gel initial water removal drying tower 2, a molecular sieve deep water removal drying tower 3, a first anisole storage tank 4, a chemical drying tower 5, and a second anisole storage tank 6 connected in series; two silica gel initial water removal drying towers 2 are arranged in parallel between the rectifying tower 1 and the molecular sieve deep water removal drying tower 3, one of which is used as a silica gel initial water removal standby tower, a switching valve 8 is arranged on the upstream main pipeline, and a moisture online detector 7 is arranged on the downstream main pipeline, and the switching valve 8 and the moisture online detector 7 are respectively connected with a controller (not shown) to realize electrical signal connection, so that the controller can be set based on the water content of the moisture online detector 7, and the switching valve 8 is switched to ensure that the water content of the anisole obtained by the initial water removal of silica gel satisfies ≤50ppm; a cooler is arranged between the chemical drying tower 5 and the second anisole storage tank 6;

[0041] The distillation tower 1 is a packed tower, which is provided with two sections of packing and feeds between towers. The packed tower adopts φ6×6θ mesh ring packing. The distillation tower 1 is equipped with a temperature sensor and a pressure sensor. The tower diameter of the distillation tower 1 is 100 mm; the silica gel primary water removal drying tower 2 is filled with silica gel particles, and the silica gel primary water removal drying tower 2 adopts a fixed bed with a bed height of 30 to 50 cm and an inner diameter of 6 to 10 cm; the molecular sieve deep water removal drying tower 3 is filled with molecular sieve particles, and the molecular sieve deep water removal drying tower 3 adopts a fixed bed with a bed height of 30 to 50 cm and an inner diameter of 10 to 15 cm;

[0042] The tops of rectifying tower 1, silica gel initial water removal drying tower 2, molecular sieve deep water removal drying tower 3, and the first anisole storage tank 4 are respectively provided with anisole inlet and the bottom is respectively provided with anisole outlet, chemical drying tower 5 is a fixed-bed reactor, the top offers the chemical drying anisole inlet, is used to feed the anisole from the first anisole storage tank 4, the bottom offers the CO gas inlet, is used to feed the CO gas required for chemical reaction, the middle part is fixedly provided with catalyst, is used to catalyze and carry out water-gas reaction in the chemical drying tower, the top offers the chemical drying waste gas outlet, is used to discharge the waste gas generated by the water-gas reaction, the bottom offers the chemical drying anisole outlet, is used to discharge the anisole for boron isotope separation whose water content is 1~3ppm, and is stored in the second anisole storage tank 6; The internal volume of chemical drying tower 5 is 150L, ​​and the ratio of height to diameter is 2.5.

[0043] Application Example 1

[0044] This application example provides a continuous deep dehydration method for anisole for boron isotope separation, using the continuous deep dehydration device described in Example 1. The continuous deep dehydration method includes the following contents:

[0045] The purity of the anisole to be dehydrated is 99.7wt% and the water content is 100ppm, which meets the requirements of purity ≥99.5wt% and water content of 80-120ppm. The product has high purity and does not need to enter the distillation tower 1 for distillation treatment, and can directly perform initial water removal on silica gel;

[0046] The anisole to be dehydrated enters the silica gel initial water removal drying tower 2 and carries out the silica gel initial water removal, the silica gel initial water removal drying tower 2 adopts fixed bed to carry out, the fixed bed is filled with 100 purpose silica gel particles, the bed height is 50cm, the internal diameter is 10cm, the anisole flow rate of the silica gel initial water removal is 50mL / min, and the water content of the anisole obtained meets≤50ppm;

[0047] The anisole completing the initial dehydration of silica gel enters the molecular sieve deep water removal drying tower 3 to carry out the deep dehydration of molecular sieve, the molecular sieve deep water removal drying tower 3 adopts fixed bed to carry out, the fixed bed is filled with 100 mesh 4A molecular sieve particles, the bed height is 50cm, and the internal diameter is 10cm, the anisole flow velocity of the molecular sieve deep dehydration is 50mL / min, and the water content initial concentration of the anisole at the outflow outlet is 8ppm, after 200min, the water content of the anisole at the outflow outlet is 10ppm, and the anisole completing the deep dehydration of the molecular sieve enters the first anisole storage tank 4 for storage.

[0048] Application Example 2

[0049] This application example provides a continuous deep dehydration method for anisole for boron isotope separation, using the continuous deep dehydration device described in Example 1. The continuous deep dehydration method includes the following contents:

[0050] Adopt common anisole industrial product, purity is 95.0wt%, water content is 1wt%, do not meet the requirement that purity ≥99.5wt%, water content is 80~120ppm, need to enter rectifying tower 1 and carry out rectification treatment, control the target temperature of rectification to be 155 ℃, the target pressure of rectification is 130Pa / m, the purity of anisole is increased to 99.6wt%, and water content is reduced to 80ppm;

[0051] The anisole after rectification enters the silica gel initial water removal drying tower 2 to carry out the silica gel initial water removal, the silica gel initial water removal drying tower 2 adopts a fixed bed, the fixed bed is filled with 200 mesh silica gel particles, the bed height is 30cm, the internal diameter is 6cm, the anisole flow rate of the silica gel initial water removal is 50mL / min, and the water content of the anisole obtained meets ≤50ppm;

[0052] The anisole that has completed the initial dehydration of silica gel enters the molecular sieve deep dehydration drying tower 3 for molecular sieve deep dehydration. The molecular sieve deep dehydration drying tower 3 adopts fixed bed, and the fixed bed is filled with 200 mesh 5A molecular sieve particles. The bed height is 50cm, and the internal diameter is 10cm. The anisole flow rate of the molecular sieve deep dehydration is 100mL / min, and the initial water content of the anisole at the outflow outlet is 7ppm. After about 100min, the outlet moisture detector of the initial dehydration drying tower detects that the water content exceeds 50ppm, and the switching valve is used to switch to a spare tower. After 200min of total dehydration, the water content of the anisole at the outflow outlet is 9ppm; The anisole that has completed the deep dehydration of the molecular sieve enters the first anisole storage tank 4 for storage.

[0053] Application Example 3

[0054] This application example provides a continuous deep dehydration method for anisole for boron isotope separation, using the continuous deep dehydration device described in Example 1. The continuous deep dehydration method includes the following contents:

[0055] Adopt common anisole industrial product, purity is 95.0wt%, water content is 1wt%, do not meet the requirement that purity ≥99.5wt%, water content is 80~120ppm, need to enter rectifying tower 1 and carry out rectification treatment, control the target temperature of rectification to be 155 ℃, the target pressure of rectification is 130Pa / m, the purity of anisole is increased to 99.6wt%, and water content is reduced to 80ppm;

[0056] The anisole after the rectification enters the silica gel initial water removal drying tower 2 to carry out the silica gel initial water removal, the silica gel initial water removal drying tower 2 adopts a fixed bed to carry out, the fixed bed is filled with 400 mesh silica gel particles, the bed height is 40cm, the internal diameter is 10cm, the anisole flow rate of the silica gel initial water removal is 50mL / min, and the water content of the anisole obtained meets≤50ppm;

[0057] The anisole completing the initial dewatering of silica gel enters the deep dewatering drying tower 3 of molecular sieve and carries out the deep dewatering of molecular sieve, the deep dewatering drying tower 3 of molecular sieve adopts fixed bed to carry out, and fixed bed is filled with 400 purpose 13X molecular sieve particles, and bed height is 30cm, and internal diameter is 15cm, and the anisole flow velocity of the deep dewatering of molecular sieve is 60mL / min, the water content initial concentration 8ppm of the flow outlet anisole, after about 100min, the outlet moisture detector of the initial dewatering drying tower detects that water content exceeds 50ppm, utilizes switching valve 8 to switch to standby tower, and after total dewatering 200min, the flow outlet anisole water content is 10ppm; The anisole completing the deep dewatering of molecular sieve enters the first anisole storage tank 4 to store, for balancing and stabilizing pipeline pressure;

[0058] Anisole from the first anisole storage tank 4 enters a chemical drying tower 5, which is a fixed reaction bed. A catalyst is loaded in the tower. Anisole is pumped into the tower from the top with a constant flow pump at a flow rate of 20 mL / min, and CO is pumped into the tower from the bottom with a pressure pump at a flow rate of 10 mL / min. Ultra-deep water removal is carried out under the action of a catalyst. The reaction temperature is controlled to be 200 ° C, the reaction pressure is 1.0 MPa, and the reaction time is 4 h. Reaction waste gas is removed from the top of the tower, and anisole is removed from the bottom of the tower and then cooled. The tower enters the second anisole storage tank 6 to obtain anisole for boron isotope separation and the water content is reduced to 1 ppm.

[0059] It should be noted that, using the continuous deep dehydration method of the present invention, once the silica gel initial dehydration and molecular sieve deep dehydration are carried out in sequence for 200 minutes of continuous deep dehydration, and the water content of anisole at the outlet meets the corresponding requirements, they are switched to another continuous deep dehydration process production line. That is, except for emergencies, the switching of the continuous deep dehydration process production line is based on whether the continuous operation time reaches 200 minutes.

[0060] The present invention adopts the continuous deep dehydration device of anisole for boron isotope separation, and the water content of anisole is gradually reduced. First, most of water and impurities in anisole with a water content of 1wt% are removed through a rectifying tower under normal pressure, and then the anisole is passed through a silica gel primary dehydration drying tower equipped with silica gel particles. After sufficient mixing, water is preliminarily adsorbed and the water content can be reduced to about 50ppm. The anisole containing trace water is further fully dehydrated through a molecular sieve deep dehydration drying tower equipped with a molecular sieve, and the water content can be reduced to about 10ppm; a storage tank can be installed between the towers for balancing and stabilizing pipeline pressure, and an online moisture detector is installed at the water outlet of the primary dehydration drying tower for monitoring the running state of the drying tower; when the water content of anisole is required to be more stringent, the anisole can be further subjected to ultra-dehydration by a chemical reaction method, that is, water gas reaction is carried out through a chemical drying tower, and the water content can be reduced to 1-3ppm.

[0061] In summary, the present invention provides a kind of continuous deep dehydration device of anisole for boron isotope separation, comprising a silica gel primary dehydration drying tower and a molecular sieve deep dehydration drying tower connected in series, anisole is subjected to two-step dehydration treatment in sequence, firstly, the anisole subjected to silica gel primary dehydration is limited to meet the conditions of purity ≥99.5wt% and water content 80~120ppm, then silica gel primary dehydration is performed, so that the water in anisole is preliminarily adsorbed by silica gel particles, the water content of anisole obtained by silica gel primary dehydration is ≤50ppm, then the anisole containing trace water is subjected to molecular sieve deep dehydration, so that the trace water is further fully dehydrated by the molecular sieve, thereby obtaining anisole for boron isotope separation and water content ≤10ppm. The continuous deep dehydration device of the present invention has simple structure and high safety, and can also further reduce production cost by means of the regeneration of silica gel particles and molecular sieve particles, so as to facilitate industrial promotion and use.

[0062] The present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the components selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0063] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0064] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0065] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A continuous deep dehydration device for anisole for boron isotope separation, characterized in that: The continuous deep dehydration device comprises a silica gel primary dehydration drying tower and a molecular sieve deep dehydration drying tower connected in series in sequence; The silica gel primary dehydration drying tower is filled with silica gel particles, and an inlet for primary dehydration anisole is provided at the top for adding anisole with a purity of ≥99.5wt% and a water content of 80-120ppm; an outlet for primary dehydration anisole is provided at the bottom, and an online moisture detector is provided at the outlet for primary dehydration anisole for online monitoring of the water content of anisole discharged from the outlet for primary dehydration anisole, so that anisole with a water content of ≤50ppm enters the molecular sieve deep dehydration drying tower; The molecular sieve deep water removal drying tower is filled with molecular sieve particles, a deep water removal anisole inlet is arranged at the top and connected to the primary water removal anisole outlet, and a deep water removal anisole outlet is arranged at the bottom for discharging anisole with a water content of ≤10ppm for boron isotope separation.

2. The continuous deep dehydration device according to claim 1, characterized in that: A distillation tower is arranged in series upstream of the silica gel primary water removal drying tower to distill industrial anisole to obtain anisole with a purity of ≥99.5wt% and a water content of 80-120ppm.

3. The continuous deep dehydration device according to claim 2, characterized in that: The distillation tower is a packed tower, which is provided with two sections of packing and feeds between the towers. Mesh ring packing.

4. The continuous deep dehydration device according to claim 2, characterized in that: The distillation tower is equipped with a temperature sensor and a pressure sensor.

5. The continuous deep dehydration device according to claim 2, characterized in that: The diameter of the distillation tower is 80-120 mm.

6. The continuous deep dehydration device according to claim 1 or 2, characterized in that: A first anisole storage tank, a chemical drying tower and a second anisole storage tank are sequentially arranged in series downstream of the molecular sieve deep water removal drying tower; The chemical drying tower is a fixed bed reactor, with a chemical drying anisole inlet at the top for introducing anisole from a first anisole storage tank; a CO gas inlet at the bottom for introducing CO gas required for a chemical reaction; a catalyst fixedly arranged in the middle for catalyzing a water gas reaction in the chemical drying tower; a chemical drying waste gas outlet at the top for discharging waste gas generated by the water gas reaction; and a chemical drying anisole outlet at the bottom for discharging anisole with a water content of 1 to 3 ppm for boron isotope separation, and storing the anisole in a second anisole storage tank.

7. The continuous deep dehydration device according to claim 6, characterized in that: The internal volume of the chemical drying tower is 100-200L, and the ratio of height to diameter is 2-3.

8. The continuous deep dehydration device according to any one of claims 1, 2 or 6, characterized in that: The silica gel primary water removal drying tower adopts a fixed bed, the bed height is 30-50 cm, and the inner diameter is 6-10 cm.

9. The continuous deep dehydration device according to any one of claims 1, 2 or 6, characterized in that: The silica gel primary water removal drying tower is connected in parallel with a silica gel primary water removal standby tower, a switching valve is arranged on the upstream main pipeline of the two parallel connections, the online moisture detector is arranged on the downstream main pipeline of the two parallel connections, and the switching valve and the online moisture detector are respectively connected with the controller to realize electrical signal connection; once the online moisture detector detects that the water content of anisole discharged from the primary water removal anisole outlet exceeds 50ppm, the controller controls the switching of the switching valve, and uses the silica gel primary water removal standby tower to continue to realize continuous dehydration.

10. The continuous deep dehydration device according to any one of claims 1, 2 or 6, characterized in that: The molecular sieve deep water removal drying tower adopts a fixed bed, the bed height is 30 to 50 cm, and the inner diameter is 10 to 15 cm.

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