A continuous deep dehydration method for anisole for boron isotope separation

Abstract

The present invention provides a continuous deep dehydration method for anisole for boron isotope separation. The method comprises the following steps: first, the anisole subjected to initial silica gel dehydration is limited to satisfy the conditions of purity ≥99.5wt% and water content 80-120ppm; then, the silica gel is subjected to initial dehydration, so that water in the anisole is initially adsorbed by silica gel particles; the water content of the anisole obtained by the initial silica gel 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 with a water content ≤10ppm. The continuous deep dehydration method of the present invention is not only simple to operate and highly safe, but also can further reduce production costs by regenerating silica gel particles and molecular sieve particles, thereby facilitating industrial promotion and use.

Description

Technical Field

[0001] The invention relates to the technical field of boron isotope separation, in particular to anisole, a complexing agent used for boron isotope separation, and especially to a continuous deep dehydration method 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, and boron nitride, all in varying concentrations. The company boasts a long industry chain and a wide range of applications, playing a significant role in alleviating global petrochemical energy shortages. Application of these products in the nuclear energy sector enables the widespread development and utilization of economical, safe, and clean nuclear energy resources.

[0003] Because 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, thermal neutron shielding materials, and particularly in boron neutron therapy for cancer treatment (BNCT). The natural abundance of boron-10 is only 19-20%, necessitating enrichment and purification of 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. The boron-10 abundance can reach 92%. This process technology has advantages due to its operation under normal temperature and pressure conditions and its high 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) are both high-value-added end-use products. Compared to the methyl and ethyl ether processes, they offer significant cost-effectiveness advantages, significantly reducing production costs. This process is currently used in the United States and Georgia.

[0005] Anisole is widely used in the fields such as pharmaceutical synthesis, dye synthesis, spices preparation as important raw material, intermediate and solvent. The anisole content water of technical grade is relatively low, generally at hundreds of 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 also required. As separated object, the raw material boron trifluoride gas of isotope boron-10 and isotope boron-11 easily reacts with water, and the hydrofluoric acid produced has extremely strong corrosiveness, and violent heat release, and by-product also easily blocks pipeline, reduces 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 ensure production safety, extend equipment service life, reduce the generation of by-product, improve production efficiency.

[0006] At present, conventional anisole dehydration method has physical adsorption method, chemical reaction method.The molecular sieve drying method in physical adsorption method, such as the preparation method of a kind of ultra-dry organic solvent disclosed in CN 112479797 A, needs to be carried out in a glove box and in a nitrogen atmosphere, and reaction conditions are harsh, and are not suitable for industrialized continuous scale production.The water gas reaction method in chemical reaction method, such as the boron isotope separation complexing agent anisole refining and purification method disclosed in CN 107573224 A, removes trace water with CO under catalytic conditions with the water reaction in anisole, although the reaction dehydration depth is large but needs to be carried out under high temperature and high pressure conditions, not only need extra reaction unit and reaction conditions are relatively harsh, in addition, the raw material that the reaction system uses is CO and one of product is H2, not only inflammable and explosive and toxicity are stronger, high to operating environment requirements.

[0007] In summary, it is necessary to provide a simple continuous deep dehydration method 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 method for anisole for boron isotope separation, comprising sequentially performing primary dehydration with silica gel and deep dehydration with molecular sieves, thereby obtaining anisole for boron isotope separation with a water content of ≤10 ppm based on a two-step dehydration process. The continuous deep dehydration method of the present invention is not only simple to operate and highly safe, but also can further reduce production costs by means of regeneration of silica gel particles and molecular sieve particles, thereby facilitating 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 method for anisole for boron isotope separation, the continuous deep dehydration method comprising the following contents:

[0011] Anisole with a purity of ≥99.5wt% and a water content of 80-120ppm is first subjected to primary water removal on silica gel to obtain anisole with a water content of ≤50ppm, and then subjected to deep water removal on molecular sieves to obtain anisole for boron isotope separation with a water content of ≤10ppm.

[0012] The continuous deep dehydration method of the present invention first limits the anisole of carrying out the initial dehydration of silica gel to meet the conditions of purity ≥99.5wt%, water content is 80~120ppm, then carries out the initial dehydration of silica gel, makes the water in the anisole be preliminarily adsorbed by silica gel particles, the water content of the anisole obtained by the initial dehydration of silica gel is ≤50ppm, then the anisole containing trace water is carried out molecular sieve deep dehydration, makes trace water be further fully dehydrated by molecular sieve, thereby obtains anisole and water content ≤10ppm for boron isotope separation. The continuous deep dehydration method of the present invention is not only simple to operate, high in safety, can also further reduce production costs by the regeneration of silica gel particles and molecular sieve particles, and is convenient to industrial promotion and use.

[0013] As a preferred technical solution of the present invention, the anisole with a purity of ≥99.5wt% and a water content of 80-120ppm comprises: anisole obtained by distilling industrial anisole.

[0014] As a preferred technical solution of the present invention, the purity of the industrial anisole is 94.5-99.5wt%, for example, 94.5wt%, 95wt%, 96wt%, 97wt%, 98wt%, 99wt%, or 99.5wt%, and the water content is 0.8-1.2wt%, for example, 0.8wt%, 0.9wt%, 1wt%, 1.1wt% or 1.2wt%, etc.

[0015] And / or, the distillation temperature is 150-155°C, that is, the temperature is controlled at around the boiling point of anisole, such as 150°C, 151°C, 152°C, 153°C, 154°C or 155°C.

[0016] And / or, the distillation pressure is 120-140 Pa / m, for example, 120 Pa / m, 125 Pa / m, 130 Pa / m, 135 Pa / m or 140 Pa / m.

[0017] As a preferred technical solution of the present invention, the continuous deep dehydration method also includes: reacting the anisole obtained by deep dehydration of the molecular sieve with CO gas in a fixed bed under the action of a catalyst to perform ultra-deep dehydration to obtain anisole for boron isotope separation with a water content of 1 to 3 ppm, for example, 1 ppm, 1.5 ppm, 2 ppm, 2.5 ppm or 3 ppm.

[0018] It should be noted that whether to perform ultra-deep water removal on the anisole obtained by deep water removal with molecular sieves to further reduce the water content of the anisole can be selected by those skilled in the art according to actual needs.

[0019] As a preferred technical solution of the present invention, the reaction temperature of the ultra-deep water removal is 150-200°C, for example, 150°C, 155°C, 160°C, 165°C, 170°C, 175°C, 180°C, 185°C, 190°C, 195°C or 200°C, etc., the reaction CO pressure is 1.0-5.0 MPa, for example, 1.0 MPa, 1.5 MPa, 2.0 MPa, 2.5 MPa, 3.0 MPa, 3.5 MPa, 4.0 MPa, 4.5 MPa or 5.0 MPa, etc., and the reaction time is 3-5 h, for example, 3 h, 3.5 h, 4 h, 4.5 h or 5 h, etc.

[0020] And / or, the catalyst is a copper-based catalyst.

[0021] As a preferred technical solution of the present invention, the silica gel for initial water removal uses silica gel particles of 100 to 400 meshes, such as 100 mesh, 150 mesh, 200 mesh, 250 mesh, 300 mesh, 350 mesh or 400 mesh.

[0022] Preferably, the regeneration method of the silica gel particles comprises: drying at 130-150° C. for 2-4 hours, and / or drying by purging with dry nitrogen.

[0023] In the present invention, the silica gel particles can be regenerated by drying at 130-150°C for 2-4 hours. The drying temperature is 130-150°C, such as 130°C, 135°C, 140°C, 145°C or 150°C, and the drying time is 2-4 hours, such as 2 hours, 2.5 hours, 3 hours, 3.5 hours or 4 hours.

[0024] As a preferred technical solution of the present invention, the anisole flow rate for the initial dehydration of the silica gel is 50 to 100 mL / min, for example, 50 mL / min, 60 mL / min, 70 mL / min, 80 mL / min, 90 mL / min or 100 mL / min.

[0025] As a preferred technical solution of the present invention, the molecular sieve deep water removal uses molecular sieve particles of 100 to 400 meshes, such as 100 mesh, 150 mesh, 200 mesh, 250 mesh, 300 mesh, 350 mesh or 400 mesh.

[0026] And / or, the molecular sieve deep water removal uses molecular sieve particles of any one type among 3A, 4A, 5A or 13X.

[0027] As a preferred technical solution of the present invention, the regeneration method of the molecular sieve particles includes: drying at 220-300° C. for 4-6 hours, and / or drying by purging with dry nitrogen.

[0028] In the present invention, the molecular sieve particles can be regenerated by drying at 220-300°C for 4-6 hours. The drying temperature is 220-300°C, such as 220°C, 240°C, 260°C, 280°C or 3000°C, and the drying time is 4-6 hours, such as 4 hours, 4.5 hours, 5 hours, 5.5 hours or 6 hours.

[0029] As a preferred technical solution of the present invention, the anisole flow rate for deep water removal through the molecular sieve is 50 to 100 mL / min, for example, 50 mL / min, 60 mL / min, 70 mL / min, 80 mL / min, 90 mL / min or 100 mL / min.

[0030] Compared with the existing technical solutions, the present invention has at least the following beneficial effects:

[0031] (1) continuous deep dehydration method of the present invention, first limit the anisole that carries out the first dehydration of silica gel to meet the condition that purity ≥99.5wt%, water content are 80~120ppm, then carry out silica gel and just dehydration, make the water in the anisole be tentatively adsorbed by silica gel particles, the water content of the anisole that silica gel just dehydrates to obtain is ≤50ppm, then the anisole that contains trace water is carried out the deep dehydration of molecular sieve, make trace water be further fully dehydrated by molecular sieve, thereby obtain anisole and water content ≤10ppm for boron isotope separation;

[0032] (2) The continuous deep dehydration method of the present invention is not only simple to operate and highly safe, but can also further reduce production costs by means of the regeneration of silica gel particles and molecular sieve particles, making it easier to promote and use in industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 Schematic diagram of a continuous deep dehydration apparatus for anisole for boron isotope separation used in Example 3 of the present invention;

[0034] In the figure: 1-distillation tower; 2-silica gel primary water removal and drying tower; 3-molecular sieve deep water removal and 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

[0035] The technical solution of the present invention will be further described below with reference to the accompanying drawings and through specific implementation methods.

[0036] To better illustrate the present invention and facilitate understanding of the technical solutions of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0037] Example 1

[0038] This embodiment provides a continuous deep dehydration method for anisole for boron isotope separation, and the continuous deep dehydration method includes the following contents:

[0039] 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 can be directly subjected to primary water removal on silica gel without the need for rectification treatment.

[0040] The initial dehydration of silica gel was carried out using a fixed bed, which was filled with 100-mesh silica gel particles, with a bed height of 50 cm and an internal diameter of 10 cm. The flow rate of anisole for the initial dehydration of silica gel was 50 mL / min, and the water content of the obtained anisole met ≤50 ppm;

[0041] The deep water removal by molecular sieve was carried out using a fixed bed, which was filled with 100-mesh 4A molecular sieve particles. The bed height was 50 cm and the inner diameter was 10 cm. The anisole flow rate for deep water removal by molecular sieve was 50 mL / min, and the initial water content of anisole at the outlet was 8 ppm. After 200 min, the water content of anisole at the outlet was 10 ppm.

[0042] Example 2

[0043] This embodiment provides a continuous deep dehydration method for anisole for boron isotope separation, and the continuous deep dehydration method includes the following contents:

[0044] Adopt common anisole industrial goods, purity is 95.0wt%, and water content is 1wt%, do not satisfy the requirement that purity 〉=99.5wt%, water content are 80~120ppm, need to carry out rectification process, the target temperature of controlling rectification is 155 ℃, and the target pressure of rectifying is 130Pa / m, and the purity of anisole is brought up to 99.6wt%, and water content is reduced to 80ppm;

[0045] The anisole after the rectification is first dehydrated by silica gel, and the first dehydration of silica gel adopts fixed bed to carry out, and the fixed bed is filled with 200 purpose silica gel particles, and the bed height is 30cm, and the internal diameter is 6cm. The anisole flow velocity of the first dehydration of silica gel is 50mL / min, and the water content of the anisole obtained meets≤50ppm;

[0046] The deep dehydration of molecular sieve was carried out using a fixed bed, which was filled with 200-mesh 5A molecular sieve particles. The bed height was 50 cm and the inner diameter was 10 cm. The anisole flow rate for deep dehydration of molecular sieve was 100 mL / min. The initial water content of anisole at the outlet was 7 ppm. After about 100 minutes, the moisture detector at the outlet of the initial dehydration drying tower detected that the water content exceeded 50 ppm. The switching valve was used to switch to the spare tower. After a total dehydration of 200 minutes, the water content of anisole at the outlet was 9 ppm.

[0047] Example 3

[0048] This embodiment provides a method for continuous deep dehydration of anisole for boron isotope separation, and the continuous deep dehydration device of anisole for boron isotope separation is used. Figure 1 As shown, the continuous deep dehydration device comprises a rectifying tower 1, a silica gel initial dehydration drying tower 2, a molecular sieve deep dehydration 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 dehydration drying towers 2 are arranged in parallel between the rectifying tower 1 and the molecular sieve deep dehydration drying tower 3, 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 electrically connected with a controller (not shown) respectively, so that the controller can be arranged 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 dehydration of silica gel satisfies ≤50ppm; a cooler is arranged between the chemical drying tower 5 and the second anisole storage tank 6; the top portion of the rectifying tower 1, the silica gel initial dehydration drying tower 2, the molecular sieve deep dehydration drying tower 3, the first anisole storage tank 4 Do not offer anisole inlet and the bottom offers anisole outlet respectively, chemical drying tower 5 is a fixed-bed reactor, top offers chemical drying anisole inlet, for feeding the anisole from the first anisole storage tank 4, bottom offers CO gas inlet, for feeding CO gas required for chemical reaction, middle part is fixedly provided with catalyst, for catalysis in chemical drying tower and carries out water gas reaction, top offers chemical drying waste gas outlet, for discharging the waste gas generated by water gas reaction, bottom offers chemical drying anisole outlet, for discharging the anisole for boron isotope separation that water content is 1~3ppm, and is stored in the second anisole storage tank 6; The bottom of described silica gel just dewatering drying tower 2 offers just dewatering anisole outlet, and moisture online detector 7 is set at described just dewatering anisole outlet, for online monitoring whether the water content of the anisole discharged by just dewatering anisole outlet is≤50ppm;

[0049] The continuous deep dehydration method comprises the following contents:

[0050] Adopt common anisole industrial goods, purity is 95.0wt%, and water content is 1wt%, do not satisfy the requirement that purity 〉=99.5wt%, water content are 80~120ppm, need to enter rectifying tower 1 and carry out rectification process, the target temperature of controlling rectifying is 155 ℃, and the target pressure of rectifying is 130Pa / m, and the purity of anisole is brought up to 99.6wt%, and water content is reduced to 80ppm;

[0051] The methyl-phenoxide after the rectification enters silica gel and just dewaters and carries out silica gel just dewatering in drying tower 2, silica gel just dewaters and drying tower 2 adopts fixed bed to carry out, and fixed bed is filled with 400 purpose silica gel particles, and bed height is 40cm, and internal diameter is 10cm, and the methyl-phenoxide flow velocity of silica gel just dewatering is 50mL / min, and the water content of the methyl-phenoxide obtained satisfies≤50ppm;

[0052] The anisole that completes the just 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, fixed bed is filled with 400 purpose 13X molecular sieve particles, bed height is 30cm, internal diameter is 15cm, the anisole flow velocity that molecular sieve dewaters is deep is 60mL / min, the water content initial concentration 8ppm of outflow anisole, after about 100min, the outlet moisture detector of just dewatering drying tower detects water content and exceeds 50ppm, utilize switching valve 8 to switch standby tower, after total dewatering 200min, outflow anisole water content is 10ppm; The anisole that completes the deep dewatering of molecular sieve enters the first anisole hold-up tank 4 and stores, for balancing and stabilizing pipeline pressure;

[0053] Anisole from the first anisole storage tank 4 enters chemical drying tower 5, chemical drying tower 5 is fixed reaction bed, catalyst is loaded in the tower, anisole utilizes constant flow pump to pump in from tower top with 20mL / min flow velocity, CO pumps in with pressure pump from the bottom with 10mL / min flow velocity, under catalyst action, carry out ultra-deep water removal, controlling reaction temperature is 200 ℃, reaction pressure is 1.0MPa, and the reaction times is 4h, reaction waste gas is excluded from tower top, anisole is excluded from postcooling at the bottom of the tower, enter the second anisole storage tank 6, obtain the anisole for boron isotope separation and water content is down to 1ppm.

[0054] This embodiment adopts Figure 1The invention discloses a continuous deep dehydration device for anisole for boron isotope separation, which reduces the water content of anisole step by step. The device first passes through a rectifying tower under normal pressure to remove most of the water and impurities in anisole with a water content of 1wt%. The device then passes through a silica gel primary dehydration drying tower equipped with silica gel particles. After thorough 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 to reduce the water content to about 10ppm. A storage tank can be installed between the towers for balancing and stabilizing pipeline pressure. An online moisture detector is installed at the water outlet of the primary dehydration drying tower to monitor the running state of the drying tower. When the water content of the 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 in a chemical drying tower to reduce the water content to 1-3ppm.

[0055] Comparative Example 1

[0056] This comparative example provides a continuous deep dehydration method for anisole for boron isotope separation. Compared with Example 1, the only difference is that silica gel particles and molecular sieve particles are mixed and then loaded into a fixed bed, that is, the initial dehydration of silica gel and the deep dehydration of molecular sieve are combined into a one-step dehydration process; the specific content is as follows:

[0057] 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 can be directly subjected to primary water removal on silica gel without the need for rectification treatment.

[0058] The fixed bed is filled with a mixture of 100-mesh silica gel particles and 100-mesh 4A molecular sieve particles. The bed height is 100 cm, the inner diameter is 10 cm, the anisole flow rate is 50 mL / min, and the initial water content of anisole at the outlet is 8 ppm. After about 120 minutes, the water content of anisole at the outlet exceeds 10 ppm, which does not meet the requirement of water content ≤ 10 ppm. It is necessary to switch to another continuous deep dehydration process production line.

[0059] In this comparative example, silica gel and molecular sieve all are mainly to remove moisture by physical adsorption, the pore of silica gel is inhomogeneous, and adsorbate is not selectivity, so water absorption is big (can reach 200% of deadweight), but water absorbing capacity (referring to the removal ability to low concentration water) is low, the pore of molecular sieve is uniform, only has adsorption capacity to the molecule less than pore diameter, therefore can selectively remove the trace water in the anisole, but adsorption capacity is less (lower than 20%).Therefore mixed words, molecular sieve reaches saturation very soon under high concentration water, promptly loses the ability of deep dehydration subsequently.

[0060] It should be noted that, using the continuous deep dehydration method of the present invention, continuous deep dehydration for 200 min, the water content of anisole at the outlet meets the corresponding requirements, and is 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 reaches 200 min.

[0061] In summary, the invention provides a kind of continuous deep dehydration method of the anisole for boron isotope separation, first limit the anisole that carries out silica gel just dehydration and meet purity ≥99.5wt%, water content is the condition of 80~120ppm, then carry out silica gel just dehydration, make the water in anisole be tentatively adsorbed by silica gel particles, the water content of the anisole that silica gel just dehydration obtains is≤50ppm, then the anisole containing trace water is carried out molecular sieve deep dehydration, make trace water be further fully dehydrated by molecular sieve, thus obtain anisole and water content≤10ppm for boron isotope separation.Continuous deep dehydration method of the present invention, not only simple to operate, high safety, can also by the regeneration of silica gel particles and molecular sieve particles, further reduce production cost, be convenient to industrial promotion and use.

[0062] While the present invention is described through the above-described embodiments to illustrate the detailed structural features of the present invention, the present invention is not limited to these detailed structural features, nor does it necessarily rely on these detailed structural features for implementation. Those skilled in the art should understand that any improvements to the present invention, equivalent replacements for selected components, additions of auxiliary components, and selection of specific embodiments, etc., fall within the scope of protection and disclosure 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, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection 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 appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0065] In addition, the 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 method for anisole for boron isotope separation, characterized in that, The continuous deep dehydration method comprises the following contents: Anisole with a purity of ≥99.5wt% and a water content of 80-120ppm is first subjected to initial dehydration on silica gel to obtain anisole with a water content of ≤50ppm, and then subjected to deep dehydration on molecular sieves to obtain anisole for boron isotope separation with a water content of ≤10ppm; The regeneration method of the silica gel particles comprises: drying at 130-150° C. for 2-4 hours, and / or drying by purging with dry nitrogen; The regeneration method of the molecular sieve particles comprises: drying at 220-300° C. for 4-6 hours, and / or drying by purging with dry nitrogen; The silica gel for initial water removal uses silica gel particles of 100-400 mesh; the anisole flow rate for the silica gel for initial water removal is 50-100 mL / min; The molecular sieve deep water removal uses molecular sieve particles of 100-400 mesh; the molecular sieve deep water removal uses molecular sieve particles of any one model among 3A, 4A, 5A or 13X; the anisole flow rate of the molecular sieve deep water removal is 50-100 mL / min.

2. The continuous deep dehydration method according to claim 1, characterized in that The anisole with a purity of ≥99.5wt% and a water content of 80-120ppm comprises anisole obtained by distilling industrial anisole.

3. The continuous deep dehydration method according to claim 2, characterized in that: The industrial anisole has a purity of 94.5-99.5 wt % and a water content of 0.8-1.2 wt %; and / or, the distillation temperature is 150-155° C.; And / or, the distillation pressure is 120-140 Pa / m.

4. The continuous deep dehydration method according to claim 1, characterized in that: The continuous deep dehydration method further comprises: reacting the anisole obtained by deep dehydration of the molecular sieve with CO gas in a fixed bed under the action of a catalyst to perform ultra-deep dehydration to obtain anisole for boron isotope separation with a water content of 1-3 ppm.

5. The continuous deep dehydration method according to claim 4, characterized in that: The reaction temperature of the ultra-deep water removal is 150-200°C, the reaction CO pressure is 1.0-5.0 MPa, and the reaction time is 3-5 hours; And / or, the catalyst is a copper-based catalyst.

Images