Refining and purifying system for ethyl p-aminobenzoate

Abstract

The utility model discloses a refining and purifying system for ethyl p-aminobenzoate, which comprises a decoloring kettle, a filter, a crystallization kettle, a centrifugal machine, an auger conveyor and a double-cone drying box, the decoloring kettle, the filter and the crystallization kettle are sequentially connected, and a discharge port of the crystallization kettle is connected with a feed port of the centrifugal machine. A discharge port of the centrifugal machine is communicated with a feed port of the double-cone drying box through an auger conveyor, a discharge port of the crystallization kettle is further connected with a feed port of the decolorizing kettle, the crystallization kettle is provided with an online detector, and the crystallization kettle, the centrifugal machine, the auger conveyor and the double-cone drying box are sequentially arranged from top to bottom. And the automation degree is high, the quality of produced products is high, the stability among batches is good, and the good application and popularization prospects are achieved.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical equipment reaction, and in particular to a refining and purification system for ethyl p-aminobenzoate. Background Art

[0002] Ethyl p-aminobenzoate, also known as benzocaine, is widely used in the production of medicines and high-end materials. In medicine, ethyl p-aminobenzoate is a non-water-soluble local anesthetic with good analgesic and antipruritic effects. It is mainly used for analgesia and antipruritic effects on ulcers, wounds and mucosal surfaces. Its ointment can be used for lubrication and analgesia of nasopharyngeal catheters, endoscopes, etc. As a highly ester-soluble local anesthetic, ethyl p-aminobenzoate easily combines with the lipid layer of the skin or mucosa and is not easy to enter the body to produce toxicity. In terms of materials, ethyl p-aminobenzoate is a protective agent that blocks sunlight ultraviolet rays and is added to plastics and coatings.

[0003] As a commonly used API and material additive worldwide, ethyl p-aminobenzoate has high market requirements for its appearance, purity, chromaticity, acidity, related substances, metal ions, drying loss and ignition residue. The original production system can no longer meet the new and higher market demands due to its backward performance. Therefore, based on a large amount of theoretical research and experiments, we upgraded the refining and purification equipment of the product, added an online product quality detection system, and adjusted the process parameters and conditions in a timely manner according to the test results; we adopted nitrogen protection for the entire process to ensure that the product will not be oxidized and discolored during the preparation process, affecting the product quality. We adopted a more scientific equipment layout method to make the material transmission smoother and more energy-saving. The utility model has high production efficiency, relatively mild reaction conditions, high degree of automation, good product quality, small waste emissions, environmental friendliness, and good social and economic value. Utility Model Content

[0004] According to the technical problems raised above, a refining and purification system for ethyl p-aminobenzoate is provided.

[0005] The technical means adopted by the utility model are as follows:

[0006] A refining and purification system for ethyl p-aminobenzoate comprises a decolorizing kettle (100), a filter (200), a crystallizing kettle (300), a centrifuge (400), an auger conveyor (500) and a double-cone drying oven (600) which are connected in sequence;

[0007] The top of the decolorization kettle is provided with a nitrogen inlet (101), an exhaust port (102), a vacuum port (103), and a decolorization kettle feed port (104); the bottom of the decolorization kettle is provided with a decolorization kettle discharge port; and a stirrer is provided in the decolorization kettle;

[0008] The filter (200) comprises a plate filter (210) and a microfilter (220) which are arranged in series, wherein a plate filter feed port (211) and a plate filter exhaust port (212) are provided at the top of the plate filter (210), and a plate filter discharge port (213) is provided at the bottom of the plate filter;

[0009] The top of the crystallization kettle (300) is provided with a crystallization kettle feed port (301), a crystallization kettle nitrogen inlet (302), and a crystallization kettle exhaust port (303); the bottom of the crystallization kettle is provided with a crystallization kettle discharge port (304); and a crystallization kettle agitator (305) and an online detector (306) are provided in the crystallization kettle;

[0010] The centrifuge 400 comprises a centrifuge body (410) and a driving device (420) for driving the centrifuge body, wherein the centrifuge body (410) is provided with a centrifuge body feed inlet (411), a centrifuge mother liquor outlet (412) and a solid material outlet (413);

[0011] The plate filter feed port (211) is connected to the decolorization kettle discharge port (105), and the plate filter discharge port (213) is connected to the crystallization kettle feed port (301) via a microfilter (220); the crystallization kettle discharge port (304) is connected to the centrifuge body feed port (411), and the solid material outlet (413) is connected to the barrel feed port (602-1) via an auger conveyor (500).

[0012] Furthermore, the discharge port (304) of the crystallization kettle (300) is connected to the feed port (104) of the decolorization kettle (100).

[0013] Furthermore, the centrifuge (400) is a bottom-discharging centrifuge.

[0014] Furthermore, the crystallization kettle (300), the centrifuge (400), the auger conveyor (500) and the double-cone drying box (600) are arranged in sequence from top to bottom.

[0015] Furthermore, the centrifuge body (410) is also provided with a centrifuge body nitrogen inlet (414).

[0016] Furthermore, the double-cone drying box 600 comprises two relatively arranged brackets (601), a cylinder (602), a double-cone drying box driving device (603), a heat medium outlet (604), a heat medium inlet (605), a double-cone drying box nitrogen inlet (606), a double-cone drying box vacuum port (607) and a controller (608); the cylinder (602) is rotatably connected between the brackets (601); the heat medium outlet (604) and the heat medium inlet (605) are arranged on the outside of the left bracket; the controller (608) is electrically connected to the cylinder (602); the double-cone drying box nitrogen inlet (606) and the double-cone drying box vacuum port (607) are arranged on the outside of the right bracket; and a cylinder material port (602-1) is provided at the top of the cylinder (602).

[0017] Compared with the prior art, the utility model has the following advantages:

[0018] The utility model can effectively avoid the situation where, after crystallization and centrifugal filtration, sampling and testing reveal that the product is unqualified, and rework is required, which causes a great waste of manpower and resources and brings unnecessary troubles to production organization and management. Online detection can be carried out while production is in progress, and necessary process disposal measures can be taken at any time, which effectively improves production efficiency. The utility model adopts nitrogen protection throughout the entire process, which effectively avoids oxidation and discoloration of the product and effectively improves the quality of the product. The utility model has high production efficiency, low production cost, high degree of automation, high quality of the products produced, good stability between batches, and has good prospects for promotion and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0020] Figure 1 The utility model provides a structural schematic diagram of a refining and purification system for ethyl p-aminobenzoate.

[0021] In the figure: 100, decolorization kettle; 200, filter; 300, crystallization kettle; 400, centrifuge; 500, auger conveyor; 600, double cone drying oven; 101, nitrogen inlet; 102, exhaust port; 103, vacuum port; 104, decolorization kettle feed port; 210, plate filter; 220, microfilter; 211, plate filter feed port; 212, plate filter exhaust port; 213, plate filter outlet; 301, crystallization kettle feed port; 302, crystallization kettle nitrogen inlet; 303, crystallization kettle exhaust port ; 304, crystallization kettle discharge port; 305, crystallization kettle agitator; 306, online detector; 410, centrifuge body; 420, drive device; 411, centrifuge body feed port; 412, centrifuge mother liquor outlet; 413, solid material outlet; 414, centrifuge body nitrogen inlet; 601, bracket; 602, cylinder; 603, double cone drying box drive device; 604, heat medium outlet; 605, heat medium inlet; 606, double cone drying box nitrogen inlet; 607, double cone drying box vacuum outlet; 608, controller. DETAILED DESCRIPTION

[0022] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments of the present invention can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0023] In order to make the purpose, technical scheme and advantages of the embodiments of the utility model clearer, the technical scheme in the embodiments of the utility model will be clearly and completely described below in conjunction with the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. The following description of at least one exemplary embodiment is actually only illustrative and is by no means a limitation on the utility model and its application or use. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the utility model.

[0024] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the utility model. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0025] Unless otherwise specifically stated, the relative arrangement, numerical expressions and numerical values ​​of the parts and steps set forth in these embodiments do not limit the scope of the utility model. At the same time, it should be clear that, for ease of description, the sizes of the various parts shown in the accompanying drawings are not drawn according to the actual proportional relationship. The technology, method and equipment known to those of ordinary skill in the relevant field may not be discussed in detail, but in appropriate cases, the technology, method and equipment should be considered as a part of the specification. In all examples shown and discussed here, any specific value should be interpreted as being merely exemplary, rather than as a limitation. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters represent similar items in the following drawings, and therefore, once a certain item is defined in an accompanying drawing, it does not need to be further discussed in subsequent drawings.

[0026] In the description of the present utility model, it needs to be understood that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, perpendicular, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present utility model and simplifying the description. Unless otherwise stated, these directional words do not indicate or imply that the device or element referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present utility model: the directional words "inside and outside" refer to the inside and outside relative to the contours of each component itself.

[0027] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used here to describe the spatial positional relationship between a device or feature and other devices or features as shown in the figure. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figure. For example, if the device in the accompanying drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below their position devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0028] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the utility model.

[0029] like Figure 1 As shown, the utility model provides a refining and purification system for ethyl p-aminobenzoate, comprising a decolorizing kettle (100), a filter (200), a crystallization kettle (300), a centrifuge (400), an auger conveyor (500) and a double-cone drying oven (600) which are connected in sequence;

[0030] The top of the decolorization kettle is provided with a nitrogen inlet (101), an exhaust port (102), a vacuum port (103), and a decolorization kettle feed port (104); the bottom of the decolorization kettle is provided with a decolorization kettle discharge port; and a stirrer is provided in the decolorization kettle;

[0031] The filter (200) comprises a plate filter (210) and a microfilter (220) which are arranged in series, wherein a plate filter feed port (211) and a plate filter exhaust port (212) are provided at the top of the plate filter (210), and a plate filter discharge port (213) is provided at the bottom of the plate filter;

[0032] The top of the crystallization kettle (300) is provided with a crystallization kettle feed port (301), a crystallization kettle nitrogen inlet (302), and a crystallization kettle exhaust port (303); the bottom of the crystallization kettle is provided with a crystallization kettle discharge port (304); and a crystallization kettle agitator (305) and an online detector (306) are provided in the crystallization kettle;

[0033] The centrifuge 400 comprises a centrifuge body (410) and a driving device (420) for driving the centrifuge body, wherein the centrifuge body (410) is provided with a centrifuge body feed inlet (411), a centrifuge mother liquor outlet (412) and a solid material outlet (413);

[0034] The plate filter feed port (211) is connected to the decolorization kettle discharge port (105), and the plate filter discharge port (213) is connected to the crystallization kettle feed port (301) via a microfilter (220); the crystallization kettle discharge port (304) is connected to the centrifuge body feed port (411), and the solid material outlet (413) is connected to the barrel feed port (602-1) via an auger conveyor (500).

[0035] The discharge port (304) of the crystallization kettle (300) is connected to the feed port (104) of the decolorization kettle (100).

[0036] The centrifuge (400) is a bottom-discharging centrifuge.

[0037] The crystallization kettle (300), the centrifuge (400), the auger conveyor (500) and the double-cone drying box (600) are arranged in sequence from top to bottom.

[0038] The centrifuge body (410) is also provided with a centrifuge body nitrogen inlet (414).

[0039] The double-cone drying box 600 comprises two relatively arranged brackets (601), a cylinder (602), a double-cone drying box driving device (603), a heat medium outlet (604), a heat medium inlet (605), a double-cone drying box nitrogen inlet (606), a double-cone drying box vacuum port (607) and a controller (608). The cylinder (602) is rotatably connected between the brackets (601), the heat medium outlet (604) and the heat medium inlet (605) are arranged on the outside of the left bracket, the controller (608) is electrically connected to the cylinder (602), the double-cone drying box nitrogen inlet (606) and the double-cone drying box vacuum port (607) are arranged on the outside of the right bracket, and a cylinder material port (602-1) is provided at the top of the cylinder (602). The general working process of the double cone dryer: first, when the equipment is in good condition, open the barrel material port 602-1, put the material into the double cone dryer 600, close the barrel material port 602-1, open the vacuum port 607 to continuously vacuum the double cone dryer 600, open the heat medium outlet 604 and the heat medium inlet 605 to heat the double cone dryer 600 to a certain temperature, and dry until the product is dry and wet. Adjust the heat medium temperature, cool down, close the heat medium outlet 604 and the heat medium inlet 605, close the vacuum port 607, open the nitrogen inlet 606 to fill the double cone dryer 600 with nitrogen to atmospheric pressure, close the nitrogen inlet 606, open the barrel material port 602-1, and discharge the material.

[0040] Solvent, ethyl para-aminobenzoate, activated carbon and other materials are added to the decolorization kettle 100 in a certain proportion, heated and stirred for decolorization and purification, filtered while hot, and the filtrate is filtered through the plate filter 210 and the microfilter 220 at two stages before entering the crystallization kettle 300. The online detector 306 of the crystallization kettle 300 performs online detection on the clarity, pH, chromaticity and key impurities of the material. If the detection is qualified, the material is cooled and crystallized, and sent to the centrifuge 400 for filtration, and then sent to the double cone dryer 600 for drying via the auger conveyor 500; if the detection is unqualified, it will be processed according to a special process flow, such as returning to the decolorization kettle 100 for secondary refining and filtration, until the detection is qualified, cooling and crystallization, centrifugal filtration and drying operations are performed to obtain the finished ethyl para-aminobenzoate.

[0041] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model, rather than to limit it. Although the utility model has been described in detail with reference to the aforementioned embodiments, ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solution deviate from the scope of the technical solution of the embodiments of the utility model.

Claims

1. A refining and purification system for ethyl p-aminobenzoate, characterized in that: It comprises a decolorizing kettle (100), a filter (200), a crystallizing kettle (300), a centrifuge (400), an auger conveyor (500) and a double-cone drying oven (600) which are connected in sequence; The top of the decolorization kettle is provided with a nitrogen inlet (101), an exhaust port (102), a vacuum port (103), and a decolorization kettle feed port (104); the bottom of the decolorization kettle is provided with a decolorization kettle discharge port; and a stirrer is provided in the decolorization kettle; The filter (200) comprises a plate filter (210) and a microfilter (220) which are arranged in series, wherein a plate filter feed port (211) and a plate filter exhaust port (212) are provided at the top of the plate filter (210), and a plate filter discharge port (213) is provided at the bottom of the plate filter; The top of the crystallization kettle (300) is provided with a crystallization kettle feed port (301), a crystallization kettle nitrogen inlet (302), and a crystallization kettle exhaust port (303); the bottom of the crystallization kettle is provided with a crystallization kettle discharge port (304); and a crystallization kettle agitator (305) and an online detector (306) are provided in the crystallization kettle; The centrifuge (400) comprises a centrifuge body (410) and a driving device (420) for driving the centrifuge body, wherein the centrifuge body (410) is provided with a centrifuge body feed inlet (411), a centrifuge mother liquor outlet (412) and a solid material outlet (413); The plate filter feed port (211) is connected to the decolorization kettle discharge port (105), and the plate filter discharge port (213) is connected to the crystallization kettle feed port (301) via a microfilter (220); the crystallization kettle discharge port (304) is connected to the centrifuge body feed port (411), and the solid material outlet (413) is connected to the barrel feed port (602-1) via an auger conveyor (500).

2. A refining and purification system for ethyl p-aminobenzoate according to claim 1, characterized in that: The discharge port (304) of the crystallization kettle (300) is connected to the feed port (104) of the decolorization kettle (100).

3. A refining and purification system for ethyl p-aminobenzoate according to claim 1 or 2, characterized in that: The centrifuge (400) is a bottom-discharging centrifuge.

4. A refining and purification system for ethyl p-aminobenzoate according to claim 1 or 2, characterized in that: The crystallization kettle (300), the centrifuge (400), the auger conveyor (500) and the double-cone drying box (600) are arranged in sequence from top to bottom.

5. A refining and purification system for ethyl p-aminobenzoate according to claim 1 or 2, characterized in that: The centrifuge body (410) is also provided with a centrifuge body nitrogen inlet (414).

6. A refining and purification system for ethyl p-aminobenzoate according to claim 1 or 2, characterized in that: The double-cone drying box (600) comprises two supports (601) arranged opposite to each other, a cylinder (602), a double-cone drying box driving device (603), a heat medium outlet (604), a heat medium inlet (605), a double-cone drying box nitrogen inlet (606), a double-cone drying box vacuum port (607) and a controller (608). The cylinder (602) is rotatably connected between the supports (601). The heat medium outlet (604) and the heat medium inlet (605) are arranged on the outside of the left support. The controller (608) is electrically connected to the cylinder (602). The double-cone drying box nitrogen inlet (606) and the double-cone drying box vacuum port (607) are arranged on the outside of the right support. The top of the cylinder (602) is provided with a cylinder material port (602-1).

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