Equipment and method for purifying s-metolachlor
By using a multi-ventilator gas distributor and agitator device during the purification of purified pyroxolamine, the problems of moisture residue and energy costs in the stripping process are solved, and high purity and low moisture products are achieved, reducing the number of products with high purity and low moisture. energy costs.
Patent Information
- Application Number
- CN202411642837.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-18
- Publication Date
- 2025-02-21
AI Technical Summary
When purifying refined erectile pyroxolamine by existing stripping methods, it will cause moisture residue, affect product quality and stability, and at the same time, the energy cost is high.
Using a purification device including a reactor, a gas distributor and a stirrer, the gas is blown out through a plurality of ventilation holes on the gas distributor, and the gas is fully in contact with the crude oil of the refined pyroxolamine through the stirrer. Remove gas phase impurities.
The purity and quality of syrupole is significantly improved, and the moisture content is reduced to below 0.05%, and the energy cost is greatly reduced.
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Figure CN119488850A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the field of chemical production and preparation, and in particular to a device and method for purifying S-isopropylamine. Background Art
[0002] S-Isopropylamine is a highly effective, low-toxic, broad-spectrum herbicide widely used in farmland, orchards, gardens and other fields. Purification is an essential step in the process of pesticide production. After desolventization, the last step of the acylation reaction of S-Isopropylamine requires further purification.
[0003] The steam stripping method currently used in industrial production is to pass water vapor into the acylation desolventizing kettle to allow the crude oil of S-isopropylamine to come into direct contact with the water vapor. The volatile impurities in the crude oil diffuse into the gas phase in a certain proportion to achieve the effect of separation and purification. Since the steam stripping method uses steam, which is accompanied by water, not only does it require an additional process - dehydration, but a small amount of water will remain in the final product, affecting the quality of S-isopropylamine. High water content will reduce the stability of S-isopropylamine and affect its efficacy; in the subsequent preparation processing, high water content may lead to unstable preparation quality, and also affect the storage and transportation safety of the original drug, increase the risk of moisture and mold, and further affect the product quality and use effect. Secondly, from the perspective of energy cost, the price of steam is much more expensive than other gases such as nitrogen, and the steam stripping method will increase the process cost of S-isopropylamine. Summary of the invention
[0004] The purification equipment and method of S-metolachlor provided in the embodiments of the present application improve the purity of the S-metolachlor finished product, the quality of the purified S-metolachlor is significantly improved, and the energy cost is reduced.
[0005] On the one hand, a purification device for S-methylpyralid is provided, comprising a reactor, a gas distributor and a stirrer, wherein the gas distributor and the stirrer are arranged in the reactor, the gas distributor is provided with at least one circle of air holes, each circle of air holes comprises a plurality of air holes, and are arranged in a circular manner on the gas distributor, the air holes are used for introducing stripping gas; the stripping gas introduced through the plurality of air holes is fully contacted with the S-methylpyralid crude oil by stirring, so as to remove gas phase impurities in the S-methylpyralid crude oil.
[0006] Preferably, the gas distributor comprises a plurality of annular ring tubes which are sequentially coiled along the bottom wall of the reactor, and the total width of the stirring blades of the stirrer is less than or equal to the diameter of the gas distributor.
[0007] Preferably, the diameter of the gas distributor is 1000mm-1100mm, and / or the radial width of each circle of the circular ring tube is 70-80mm, and / or the diameter of the ventilation hole of the circular ring tube is 10mm-15mm.
[0008] On the other hand, a method for purifying S-metolachlor is provided, the method comprising:
[0009] After the crude S-isopropylamine oil is prepared, a stripping gas is introduced into the reactor through a gas distributor, wherein the gas distributor is provided with at least one circle of vent holes, each circle of vent holes includes a plurality of vent holes, and the vent holes are arranged in a circumferential manner on the gas distributor;
[0010] Then, the stripping gas introduced through the plurality of vents is stirred by a stirrer above the gas distributor to remove gas phase impurities in the crude isopropylamine oil.
[0011] Preferably, the stripping gas introduced is nitrogen.
[0012] Preferably, the nitrogen gas inlet pressure ranges from 0.1 MPa to 0.2 MPa.
[0013] Preferably, the nitrogen gas is introduced for no less than 1 h.
[0014] Preferably, the nitrogen introduction time is 2 h.
[0015] Preferably, the reactor temperature is maintained in the range of 95°C to 105°C.
[0016] Preferably, the gas phase impurities removed include chloroacetyl chloride and / or chiral amines.
[0017] Through repeated experimental verification, it was found that the purification scheme of S-metolachlor provided in the embodiment of the present application significantly improved the purity of the produced S-metolachlor, and could ensure that the water content of the S-metolachlor finally obtained was low. The purity of the S-metolachlor finally achieved reached more than 99%, and the water content was reduced to less than 0.05%. It can be seen that compared with the traditional purification process, the quality of the purified S-metolachlor was significantly improved, and since the cost of nitrogen is much lower than that of steam, the energy cost is also reduced. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 1 is a schematic diagram of the structure of a purification device for S-metolachlor provided in an embodiment of the present application;
[0019] Figure 2 It is a schematic diagram of the structure of a gas distributor in the S-metolachlor purification equipment provided in an embodiment of the present application;
[0020] Figure 3It is a schematic diagram of the purification flow of S-isopropylamine provided in the examples of the present application. DETAILED DESCRIPTION
[0021] In order to make the technical solutions and beneficial effects of the present application more obvious and easy to understand, the following is a detailed description by listing specific embodiments. The drawings are not necessarily drawn to scale, and local features may be enlarged or reduced to more clearly show the details of the local features; unless otherwise defined, the technical and scientific terms used herein have the same meanings as those in the technical field to which the present application belongs.
[0022] In the description of the present application, the terms "upper", "lower", "top", "bottom", "inside", "outside", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings. They are only for the convenience of simplifying the description of the present application and do not indicate that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and should not be understood as a limitation on the present application.
[0023] In addition, in the description of the present application, the meaning of "multiple" is at least two, such as two, three, etc.; the meaning of "several" is at least one, such as one, two, three, etc.; unless otherwise clearly and specifically defined. The purpose of the terms used herein is only to describe specific embodiments and is not intended to be a limitation of the present application. When used herein, the singular forms "one", "an" and "said / the" are also intended to include plural forms, unless the context clearly indicates otherwise. It should also be understood that the terms "compose" and / or "include", when used in this specification, determine the presence of the features, integers, steps, operations, elements and / or parts, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, parts and / or groups. When used herein, the term "and / or" includes any and all combinations of the relevant listed items.
[0024] In order to thoroughly understand the present application, detailed steps and detailed structures will be proposed in the following description to illustrate the technical solution of the present application. The preferred embodiments of the present application are described in detail as follows, but in addition to these detailed descriptions, the present application may also have other implementation methods. In the following description, a large number of specific details are given in order to provide a more thorough understanding of the present application. However, it is obvious to those skilled in the art that the present application can be implemented without one or more of these details. In other examples, in order to avoid confusion with the present application, some technical features known in the art are not described; that is, all features of the actual embodiments are not described here, and the known functions and steps are not described in detail.
[0025] Unless otherwise defined, the technical and scientific terms used in this application have the same meaning as those in the technical field to which this application belongs. The experimental methods in the following examples where specific conditions are not specified are usually carried out under conventional experimental conditions. The reagents and raw materials used in this application are commercially available unless otherwise specified. If specific techniques or conditions are not specified in the following examples, they are usually carried out according to the conventional techniques or conditions described in the literature in this area, or according to the product instructions and the conditions recommended by the manufacturer. The numerical ranges in the following examples all include the endpoint values.
[0026] In order to avoid the various disadvantages caused by traditional steam stripping purification, the inventors of the present application first considered adopting the stripping method. The so-called stripping method is a method for removing dissolved gases and certain volatile substances in the liquid phase. By passing gas (carrier gas) into the liquid phase, the dissolved gases and volatile substances in the liquid phase pass through the gas-liquid interface and transfer to the gas phase, thereby achieving the purpose of removing impurities.
[0027] However, the inventors found that although the stripping method does not have the problem of moisture affecting quality and cost, there is a problem of limited purity improvement. This is because during the stripping process, the gas needs to be passed into the reactor. The existing gas-passing equipment generally uses a straight pipe to pass to the bottom, which can ensure that the gas is passed into the reactor and contacts with the material. However, although the linear pipeline can ensure that the gas is passed into the reactor and contacts with the material, there are also some problems. Since there is only one gas outlet for the linear pipeline, the gas is not in uniform contact with the material in the reactor, which affects the effect of the stripping method purification, making the purity improvement of the final product have great limitations and difficulties.
[0028] To this end, the present application provides a new type of stripping gas introduction device through improvement, as well as a stripping method that allows the stripping gas to fully and evenly contact with the crude oil of S-methylpropionate to be purified, and verifies the appropriate stripping gas pressure, introduction time parameters and temperature range of the reactor through experiments, so that the final purity of S-methylpropionate reaches more than 99%, and the moisture content is reduced to less than 0.05%. Compared with traditional stripping methods and steam stripping methods, the quality of the purified S-methylpropionate is significantly improved, and the energy cost is reduced.
[0029] The following is a detailed description of the equipment and method for improving the purity of S-isopropylamine provided in the embodiments of the present application in conjunction with specific embodiments.
[0030] Example 1
[0031] Combination Figures 1 to 3This embodiment provides a device for improving the purity of S-isopropylamine, including a reactor, a gas distributor and an agitator, wherein the gas distributor and the agitator are both arranged in the reactor. The gas distributor is provided with at least one circle of vents, each circle of vents includes a plurality of vents, and is arranged in a circumferential manner on the gas distributor, and the vents are used to introduce stripping gas. Since a plurality of vents are provided in the gas distributor, the stripping gas can be introduced at multiple angles, so that the stripping gas introduced into the reactor can fully contact with the prepared S-isopropylamine crude oil (i.e., crude S-isopropylamine), and the stripping gas directly contacts the S-isopropylamine crude oil to be purified as a carrier gas, and the impurities in the crude oil are transferred to the gas phase, which can be discharged illustratively through the tail gas emission device provided in the desolventizing reactor, and the gas phase impurities can be transported to subsequent treatment processes, such as being transported to the waste gas incinerator of the three waste removal plant.
[0032] This design of stripping gas introduction is obviously much better than the conventional linear ventilation pipe with only one outlet hole in terms of gas introduction effect, reaction contact effect in the kettle and the stripping effect directly caused. In a preferred embodiment, the gas distributor is arranged at the bottom of the desolventizing kettle, that is, after the acylation and desolventizing are completed during the preparation of S-metolachlor, the prepared S-metolachlor crude oil can be directly purified.
[0033] In some preferred embodiments, a stripping regulating valve is provided on the ventilation pipe of the stripping gas, and the pressure and flow parameters of the required stripping gas can be adjusted by adjusting the valve, so as to achieve a better stripping effect by applying the control and adjustment function of different stripping scenes. In a preferred embodiment, a tail gas regulating valve is also provided on the tail gas discharge device drawn from the reactor or the desolventizing kettle, so as to adjust and control the gas phase impurities blown out to discharge more satisfactorily, while maintaining the balance of the stripping reaction in the reactor. In addition, in order to achieve uniform stirring of the gas introduced at multiple angles on the basis of optimizing the stripping gas introduction mode, an agitator is provided above the gas distributor for stirring the stripping gas introduced by multiple vents, so as to more uniformly and fully remove the gas phase impurities in the crude oil of S-isopropylamine. In some preferred embodiments, nitrogen or any other possible gas (such as air, etc.) can be used as the stripping gas. In some preferred embodiments, the gas phase impurities removed include chloroacetyl chloride and / or chiral amines, or any other gas phase impurities that may be produced, and the present application embodiment is not particularly limited to this.
[0034] In some preferred embodiments, Figure 2As shown, the gas distributor includes a plurality of ring tubes which are arranged in sequence along the bottom wall of the reactor in a coiled manner, and the total width D of the stirring blades of the agitator is less than or equal to the diameter d of the gas distributor, so that the stripping gas introduced into all the air holes on the gas distributor can be uniformly contacted with the crude isopropylamine oil through the stirring action of the stirring blades of the agitator, thereby achieving a more uniform stripping and purification effect.
[0035] In some preferred embodiments, Figure 1 As shown, the diameter d of the gas distributor is 1000mm-1100mm, so the total width D of the stirring blades of the agitator can be 1000mm-1100mm, or less than 1100mm. In some preferred embodiments, the radial widths a, b, and c of each circle of circular ring tubes can be the same or different, and can be set in a variety of ways as needed, which is not particularly limited in the embodiments of the present application. In some preferred embodiments, the width range of the radial widths a, b, and c of each circle of circular ring tubes is 70-80mm. In some preferred embodiments, the vent aperture r of the gas distributor can be specifically set as needed, and the size of the vent aperture r of each circle can be the same or different, which is not particularly limited in the embodiments of the present application. For example, the vent aperture r of each circle of circular ring tubes can be set in the range of 10mm-15mm.
[0036] Example 2
[0037] Prior to purification, crude S-metolachlor oil is prepared or prepared.
[0038] The specific preparation process is as follows:
[0039] First, methoxypropanol is dehydrogenated to generate methoxyacetone at 260°C in the presence of a catalyst, and then methoxyacetone is reacted with 2-methyl-6-ethylaniline in an organic solvent to generate imine compounds at a reaction temperature of 100-120°C. The imine compounds are hydrogenated to generate chiral amines at a reaction temperature of 100°C and a pressure of 60MPa;
[0040] Then, chiral amine and chloroacetyl chloride are used as raw materials (wherein the feed ratio of chiral amine to chloroacetyl chloride is 1:1.1-1.3), sodium hydroxide is used as an acid-binding agent, the reaction temperature is controlled below 45°C, and the reaction is carried out in the presence of an organic solvent to generate crude isopropylamine oil.
[0041] It should be noted that in this embodiment and the following embodiments 2-5, any possible preparation process can be used for the production and preparation process of the refined metolachlor crude oil or refined metolachlor crude oil to be purified, and the embodiments of the present application are not particularly limited.
[0042] The specific purification process is as follows:
[0043] After the acylation and desolventization of S-isopropylamine were completed, the kettle temperature was maintained at 98°C, the stirring speed of the kettle was 80r / min, the nitrogen introduction pressure was 0.2MPa, nitrogen was introduced for 1h, and the tail gas emission device was opened at the same time. After the stripping was completed, the material was discharged to the S-isopropylamine finished product tank. Sampling and analysis showed that the S-isopropylamine content was 99.2% and the moisture content was 0.04%.
[0044] Example 3
[0045] The specific preparation process of S-isopropylamine is the same as that in Example 2.
[0046] After the acylation and desolventization of S-isopropylamine were completed, the kettle temperature was maintained at 100°C, the stirring speed of the kettle was 85r / min, the nitrogen introduction pressure was 0.1MPa, and nitrogen was introduced for 2h. At the same time, the tail gas emission device was opened, and the material was discharged to the S-isopropylamine finished product tank after the stripping was completed. Sampling and analysis showed that the S-isopropylamine content was 99.4% and the moisture content was 0.02%.
[0047] Example 4
[0048] The specific preparation process of S-isopropylamine is the same as that in Example 2.
[0049] After the acylation and desolventization of S-isopropylamine were completed, the kettle temperature was maintained at 102°C, the stirring speed of the kettle was 100r / min, the nitrogen introduction pressure was 0.2MPa, nitrogen was introduced for 1h, and the tail gas emission device was opened at the same time. After the stripping was completed, the material was discharged to the S-isopropylamine finished product tank. Sampling and analysis showed that the S-isopropylamine content was 99.1% and the moisture content was 0.05%.
[0050] Example 5
[0051] The specific preparation process of S-isopropylamine is the same as that in Example 2.
[0052] After the acylation and desolventization of S-isopropylamine were completed, the kettle temperature was maintained at 105°C, the stirring speed of the kettle was 90r / min, the nitrogen introduction pressure was 0.1MPa, and nitrogen was introduced for 2h. At the same time, the tail gas emission device was opened. After the stripping was completed, the material was discharged to the finished product tank. After sampling and analysis, the S-isopropylamine content was 99.5% and the moisture content was 0.01%.
[0053] Comparative Example 1
[0054] After the acylation and desolventization of S-isopropylamine was completed, steam was introduced for 1 hour, and the stirring speed of the kettle was 85 r / min. After the stripping was completed, the material was discharged to the finished product tank. After sampling and analysis, the content of S-isopropylamine was 98% and the moisture content was 0.1%.
[0055] Comparative Example 2
[0056] After the acylation and desolventization of S-isopropylamine was completed, steam was introduced for 1 hour, and the stirring speed of the kettle was 90 r / min. After the stripping was completed, the material was discharged to the finished product tank. After sampling and analysis, the content of S-isopropylamine was 97.5% and the moisture content was 0.2%.
[0057] Comparative Example 3
[0058] After the acylation and desolventization of S-isopropylamine was completed, steam was introduced for 2 hours, and the stirring speed of the kettle was 70 r / min. After the stripping was completed, the material was discharged to the finished product tank. After sampling and analysis, the content of S-isopropylamine was 96.8% and the moisture content was 0.3%.
[0059] In the experimental results test of the above-mentioned Examples 2-5 and Comparative Examples 1-2, the HG / T 5425-2018 standard was implemented for the detection of S-metolachlor crude oil, and the S-metolachlor crude oil content was determined by the gas chromatography internal standard method, and the following experimental results data were obtained.
[0060] Table 1 Purity and water content of purified S-isopropylamine in Examples 2-5 and Comparative Examples 1-2
[0061]
[0062] Through repeated verification of the embodiments and comparative examples, combined with the comparison data of the experimental results of the purity content and water content of S-metolachlor, it can be seen that the S-metolachlor purification scheme provided in the embodiments of the present application significantly improves the purity of the produced S-metolachlor, and can ensure that the water content of the S-metolachlor finally obtained is low. The purity of the S-metolachlor finally achieved reaches more than 99%, and the water content is reduced to less than 0.05%. It can be seen that compared with the traditional purification process, the quality of the purified S-metolachlor is significantly improved, and since the cost of nitrogen is much lower than that of steam, the energy cost is also reduced.
[0063] It should be understood that the above embodiments are exemplary and are not intended to include all possible implementations included in the claims. Various modifications and changes may be made on the basis of the above embodiments without departing from the scope of the present disclosure. Similarly, the various technical features of the above embodiments may be arbitrarily combined to form other embodiments of the present application that may not be explicitly described. Therefore, the above embodiments only express several implementations of the present application and do not limit the scope of protection of the patent of this application.
Claims
1. A purification device for S-metolachlor, characterized in that: The invention comprises a reactor, a gas distributor and a stirrer, wherein the gas distributor and the stirrer are arranged in the reactor, the gas distributor is provided with at least one circle of air holes, each circle of air holes comprises a plurality of air holes, and are arranged in a circumferential manner on the gas distributor, and the air holes are used for introducing stripping gas; the stirrer is located above the gas distributor, and the stripping gas introduced through the plurality of air holes is stirred so as to fully contact with the S-isopropylamine crude oil, so as to remove gas phase impurities in the S-isopropylamine crude oil.
2. The S-metolachlor purification equipment according to claim 1, characterized in that: The gas distributor comprises a plurality of annular ring tubes which are arranged in sequence along the bottom wall of the reactor in a coiled manner, and the total width of the stirring blades of the stirrer is less than or equal to the diameter of the gas distributor.
3. The S-metolachlor purification equipment according to claim 2, characterized in that: The diameter of the gas distributor is 1000mm-1100mm, and / or the radial width of each circle of the circular ring tube is 70-80mm, and / or the diameter of the ventilation hole of the circular ring tube is 10mm-15mm.
4. A method for purifying S-metolachlor, characterized in that: The method comprises: After the crude S-isopropylamine oil is prepared, a stripping gas is introduced into the reactor through a gas distributor, wherein the gas distributor is provided with at least one circle of vent holes, each circle of vent holes includes a plurality of vent holes, and the vent holes are arranged in a circumferential manner on the gas distributor; Then, the stripping gas introduced through the plurality of vents is stirred by a stirrer above the gas distributor to remove gas phase impurities in the crude isopropylamine oil.
5. The method for purifying S-metolachlor according to claim 4, characterized in that: The stripping gas introduced is nitrogen.
6. The method for purifying S-metolachlor according to claim 5, characterized in that: The pressure range of nitrogen inlet pressure is 0.1MPa-0.2MPa.
7. The method for purifying S-metolachlor according to claim 6, characterized in that: The nitrogen gas introduction time should be no less than 1h.
8. The method for purifying S-metolachlor according to claim 7, characterized in that: The nitrogen gas introduction time was 2 h.
9. The method for purifying S-metolachlor according to claim 4, characterized in that: The reactor temperature is maintained in the range of 95°C to 105°C.
10. The method for purifying S-metolachlor according to claim 4, characterized in that: Gas phase impurities removed include chloroacetyl chloride and / or chiral amines.