Device for separating trimethylamine from betaine

Abstract

The utility model is applicable to the technical field of continuous chromatographic separation, and provides a device for separating trimethylamine from betaine, 12 separation units are arranged in the device, each separation unit is filled with chromatographic separation resin, the device comprises an elution area, an elution area, a feeding area, a product separation area and a top water area, the device is connected with a betaine product tank, an intermediate tank and a trimethylamine tank through pipelines; the inlet end of the betaine product tank is connected with the elution area through a pipeline, the outlet end of the betaine product tank is connected with the elution area through a pipeline, and the inlet end and the outlet end of the intermediate tank are respectively connected with the feeding area and the product separation area through pipelines; and the inlet end and the outlet end of the trimethylamine tank are respectively connected with the product separation area and the top water area through pipelines. According to the scheme, procedures are integrated, and meanwhile the production period is shortened; errors caused by manual operation are reduced; and continuous operation and continuous discharging are realized.

Description

Technical Field

[0001] The utility model belongs to the technical field of continuous chromatographic separation, and particularly relates to a device for separating trimethylamine from betaine. Background Technique

[0002] Betaine, also known as trimethylamine ethyl ester, betaine, trimethylammonium inner salt, is a quaternary ammonium derivative of glycine and a class of nitrogen-methyl compounds or trimethyl inner salts formed by replacing the hydrogen on the amino group of amino acids with methyl groups. Adding betaine to feed can protect vitamins in the feed. The feed can withstand high temperatures, has a long storage period, can greatly improve the utilization rate of the feed, and can also reduce costs.

[0003] Traditional betaine is all feed-grade betaine, and the preparation methods are as follows:

[0004] (1) Extraction method: The mother liquor of sugar beet contains 12%-15% betaine and can be directly recovered. Heat 300 parts of the mother liquor to 50 °C, add 80 parts of calcium chloride, stir for a certain time and then filter while it is hot. The filtrate is acidified with hydrochloric acid and cooled to 20-30 °C for crystallization. After separation and drying, about 30 parts of betaine are obtained.

[0005] (2) Synthesis method: It is obtained by quaternization of chloroacetic acid and trimethylamine. Neutralize 195 parts of 48.6% aqueous chloroacetic acid solution with 16% sodium hydroxide solution of Chemicalbook to form sodium chloroacetate solution, then mix it with 360 parts of 16.4% trimethylamine solution, aerate for 1 h at 50 °C, and aerate for another 1 h at 80 °C. After dilution of the reactant, it is adsorbed by ion resin (Dowex-50-8), and the betaine solution is eluted with ammonia water. Then it is concentrated under vacuum and crystallized to obtain the finished product.

[0006] Feed-grade betaine needs to remove trimethylamine and is a product of chemical synthesis. Using trimethylamine as the raw material, after synthesis, desalination is carried out by electrodialysis, and then it is evaporated, concentrated and spray-dried to obtain the product. Trimethylamine is gaseous at room temperature and is easily soluble in water. There is still 20-30 ppm of trimethylamine residue in the final dry powder, and the stench is heavy, so it can only be used as feed. However, for food-grade and pharmaceutical-grade betaine, the trimethylamine residue is required to be <5 ppm.

[0007] In summary, most of the existing preparation methods for food-grade and pharmaceutical-grade betaine have disadvantages such as complicated steps, complex operations, and high costs, and cannot meet the requirements. Content of the Utility Model

[0008] The purpose of the utility model is to provide a device for separating trimethylamine from betaine to solve the problems in the above background technique.

[0009] To achieve the above object, the present utility model provides the following technical solution: A device for separating trimethylamine from betaine, the device is internally provided with 12 separation units, and each of the separation units is filled with chromatographic separation resin. The device includes an elution zone, an elution extraction zone, a feeding zone, a product separation zone, and a top water zone. The device is connected to a betaine product tank, an intermediate tank, and a trimethylamine tank through pipelines;

[0010] The inlet end of the betaine product tank is connected to the elution zone through a pipeline, the outlet end of the betaine product tank is connected to the elution extraction zone through a pipeline, the inlet end and the outlet end of the intermediate tank are respectively connected to the feeding zone and the product separation zone through pipelines, and the inlet end and the outlet end of the trimethylamine tank are respectively connected to the product separation zone and the top water zone through pipelines.

[0011] Preferably, the elution zone, the elution extraction zone, the feeding zone, the product separation zone, and the top water zone are arranged in sequence along the circumferential direction.

[0012] Preferably, the elution zone includes 3 separation units and adopts a forward series feeding method, and pure water is used to wash the betaine on the resin into the betaine product tank.

[0013] Preferably, the elution extraction zone includes 3 separation units and adopts a forward series feeding method. The trimethylamine preferentially eluted from the resin column is pushed backward by the betaine in the betaine product tank. When the resin column moves forward, there is no longer trimethylamine on the resin column, and the outlet liquid enters the intermediate tank.

[0014] Preferably, the feeding zone includes 1 separation unit and adopts a forward feeding method. The feeding liquid is a mixed liquid of betaine and trimethylamine, and the outlet liquid enters the intermediate tank.

[0015] Preferably, the product separation zone includes 4 separation units and adopts a forward feeding method. The feeding liquid is the mixed liquid in the intermediate tank, and separation is carried out by using the different residence times of betaine and trimethylamine on the resin. The outlet liquid enters the trimethylamine tank.

[0016] Preferably, the top water zone includes 1 separation unit and adopts a reverse feeding method. The liquid in the trimethylamine tank is used to push the pure water in the separation unit out of the system for reuse.

[0017] Preferably, the feeding speeds of both the elution zone and the product separation zone are 80 - 100 mL / min.

[0018] Preferably, the feeding speed of the elution extraction zone is 50 - 70 mL / min.

[0019] Preferably, the feeding speed of the feeding zone is 10 - 30 mL / min.

[0020] Preferably, the feeding speed of the top water area is 40-60 mL / min.

[0021] Preferably, the filling amount of each separation unit is 1-2 L.

[0022] The utility model has at least the following beneficial effects:

[0023] The utility model provides a device for separating trimethylamine from betaine, which integrates processes, shortens the production cycle, reduces errors caused by manual operation, and operates continuously and discharges continuously. Description of the Drawings

[0024] Figure 1 It is a schematic diagram of the overall structure of the utility model. Detailed Embodiments

[0025] Next, the technical solutions in the embodiments of the utility model will be clearly and completely described in conjunction with the drawings in the embodiments of the utility model. Obviously, the described embodiments are only a part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the utility model.

[0026] Embodiment

[0027] Please refer to Figure 1 , the utility model provides a technical solution: a device for separating trimethylamine from betaine, with 12 separation units built-in, and chromatographic separation resin is filled inside each separation unit. The device includes an elution area, an elution extraction area, a feeding area, a product separation area, and a top water area. The device is connected with a betaine product tank, an intermediate tank, and a trimethylamine tank through pipelines;

[0028] The inlet end of the betaine product tank is connected with the elution area through a pipeline, and the outlet end of the betaine product tank is connected with the elution extraction area through a pipeline. The inlet end and the outlet end of the intermediate tank are respectively connected with the feeding area and the product separation area through pipelines. The inlet end and the outlet end of the trimethylamine tank are respectively connected with the product separation area and the top water area through pipelines.

[0029] The elution area, the elution extraction area, the feeding area, the product separation area, and the top water area are arranged in sequence along the circumferential direction.

[0030] The elution area contains 3 separation units and adopts a forward series feeding method to wash the betaine on the resin into the betaine product tank with pure water.

[0031] The elution zone contains 3 separation units and adopts a forward series feeding method. Using the betaine in the betaine product tank, the trimethylamine that comes out first on the resin column is pushed backward, so that when the resin column moves forward, there is no trimethylamine on the resin column, and the outlet liquid enters the intermediate tank.

[0032] The feeding zone contains 1 separation unit and adopts a forward feeding method. The feeding liquid is a mixed liquid of betaine and trimethylamine, and the outlet liquid enters the intermediate tank.

[0033] The product separation zone contains 4 separation units and adopts a forward feeding method. The feeding liquid is the mixed liquid in the intermediate tank, and separation is carried out by utilizing the different residence times of betaine and trimethylamine on the resin. The outlet liquid enters the trimethylamine tank.

[0034] The top water zone contains 1 separation unit and adopts a reverse feeding method. Using the liquid in the trimethylamine tank, the pure water in the separation unit is pushed out of the system for reuse.

[0035] The feeding speeds of the elution zone and the product separation zone are both 80 - 100 mL / min; the feeding speed of the elution zone is 50 - 70 mL / min; the feeding speed of the feeding zone is 10 - 30 mL / min; the feeding speed of the top water zone is 40 - 60 mL / min.

[0036] The filling amount of each separation unit is 1 - 2 L.

[0037] This patent adopts an advanced separation method of a continuous chromatography separation device. The improved production method process is designed as follows:

[0038] Betaine and trimethylamine mixed liquid - raw material tank - continuous chromatography separation device - betaine - enters the downstream process section.

[0039] In this patent, the betaine, trimethylamine, and mixed liquid - pass through the separation units in the continuous chromatography separation device filled with chromatographic separation. In the units of the continuous chromatography separation device, according to the differences in the interactions between betaine and trimethylamine on the resin, etc., the effluent is the product betaine, and the exchanged resin will enter the top water zone as the system rotates. After reverse water flushing in the top water zone, the separation column can continue to work.

[0040] The continuous chromatography separation device technology used in this patent can achieve continuous feeding and continuous product output, completely revolutionize the traditional chemical reaction method, and also eliminate multiple intermediate links in the traditional production method. At the same time, due to the continuous operation of the continuous chromatography separation device and the sequential switching of each fluid distribution valve, each separation unit will pump in liquids of different media in sequence according to the method design, such as raw materials, water, different chemical reagents, etc.

[0041] Such as Figure 1As shown in the figure, this patent uses chromatographic separation resin with a designed processing capacity of 1.28 L / H. According to the characteristics of betaine itself, the filling amount of each resin is 2 L. It is divided into the following segmented areas:

[0042] (1) Product elution area (1 - 3#): 1 - 3# is the water inlet area. Pure water is fed in a positive direction with a feeding speed of 100 ml / min. The outlet of 3# is betaine. It is necessary to detect the refractive index at the outlet of the 1# resin column before transfer to ensure that the betaine is eluted cleanly.

[0043] (2) Product extraction area (4 - 6#): It adopts a series positive feeding method. Its outlet and the outlet of 7# are combined into the inlet of 8# with a feeding speed of 60 ml / min. It is necessary to detect that there is no trimethylamine at the outlet of the 4# resin column before transfer.

[0044] (3) Feeding area (7#): The feed is a mixed solution of betaine and trimethylamine with a feeding speed of 20 ml / min.

[0045] (4) Product separation area (8 - 11# units): The feed is a mixed solution of the outlet of 6# and the outlet of 7#. The feed is in a series positive feeding method with a feeding flow rate of 80 ml / min. The discharge is a mixed solution of betaine and trimethylamine.

[0046] (5) Top water area (12#): This area is fed in a reverse direction with a feeding flow rate of 50 ml / min. The outlet of 12# is pure water. It is necessary to detect the refractive index at the outlet of 12# before transfer.

[0047] Result analysis

[0048] (1) Product yield

[0049] In this production method, the continuous chromatographic separation device technology replaces the functions of the original chemical production method, and betaine products are obtained through continuous operation and production. As shown in Table 1.

[0050] Table 1: Experimental data of continuous chromatographic separation of betaine

[0051]

[0052]

[0053] The basic principle, main features and advantages of the present utility model have been shown and described above. For those skilled in the art, it is obvious that the present utility model is not limited to the details of the above exemplary embodiments, and can be implemented in other specific forms without departing from the spirit or basic features of the present utility model. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present utility model is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be embraced within the present utility model, and any reference signs in the claims should not be regarded as limiting the claims involved.

[0054] Although the embodiments of the present utility model have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of the present utility model. The scope of the present utility model is defined by the appended claims and their equivalents.

Claims

1. A device for separating trimethylamine from betaine, characterized in that: The device has 12 separation units built in, each of which is filled with chromatographic separation resin, and includes an elution zone, an elution zone, a feed zone, a product separation zone and a top water zone. The device is connected to a betaine product tank, an intermediate tank and a trimethylamine tank through pipelines; The inlet end of the betaine product tank is connected to the elution zone through a pipeline, the outlet end of the betaine product tank is connected to the elution zone through a pipeline, the inlet end and outlet end of the intermediate tank are connected to the feed zone and the product separation zone through pipelines, respectively, and the inlet end and outlet end of the trimethylamine tank are connected to the product separation zone and the top water zone through pipelines, respectively.

2. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The elution zone, stripping zone, feed zone, product separation zone and top water zone are arranged in sequence along the circumferential direction.

3. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The elution zone comprises three separation units and adopts a forward series feeding mode.

4. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The stripping zone comprises three separation units and adopts a forward series feeding mode.

5. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The feed zone includes one separation unit and adopts a forward feeding method.

6. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The product separation zone includes 4 separation units and adopts a forward feeding method.

7. The device for separating trimethylamine from betaine according to claim 1, characterized in that: The top water zone includes one separation unit and adopts a reverse feeding method.

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