Synthesizer for medium-carbon alcohol alkoxide

Abstract

The utility model discloses a synthesis device of medium-carbon alcohol alkoxide, which comprises a reaction kettle, the reaction kettle is connected with a solvent receiving tank through a condenser, and the reaction kettle is also connected with a cooling and heating circulation all-in-one machine through a reaction kettle jacket coil; a solid feeding hole of the reaction kettle is connected with a solid raw material storage tank through a scraper type solid conveyor; a liquid raw material feeding hole of the reaction kettle is connected with a liquid raw material dripping tank through a peristaltic pump; and a solvent feeding hole of the reaction kettle is connected with a solvent tank through a solvent material conveying pump. When the synthesis device is used for preparing a product, the process is simple, the reaction process is carried out under mild conditions and normal pressure, and the reaction time is short; the device combination is reasonable, the equipment requirement is low, the obtained free alkali is low, the solvent can be recycled and reused, and the product is easy to store.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical equipment, relates to medium-carbon alcohol alkoxide, and particularly relates to a synthesis device for medium-carbon alcohol alkoxide. Background Art

[0002] The molecular general formula of medium-carbon alcohol alkoxide is R-O-M, where R refers to an alkyl group containing 5-9 carbon atoms, and M is an alkali metal, mainly sodium or potassium. Due to the relatively strong electronegativity of the oxygen atom, alcohol alkali metal salts often show a certain polarity, have a certain solubility in organic solvents, especially alcohols, and also possess some characteristics of covalent compounds. They are often used as organic synthesis intermediates, pharmaceutical intermediates or catalysts, etc., and are important raw materials in the fine chemical, pesticide and pharmaceutical industries.

[0003] Traditional methods for synthesizing medium-carbon alcohol alkoxide mainly include the metal method, the alkali method, the alkali metal amide method, the alcohol exchange method, etc. The metal method is a direct reaction between alcohol and alkali metal, and a high-boiling inert solvent is added to raise the reaction temperature above the melting point of potassium; the alkali method is a reaction between alcohol and alkali metal hydroxide, and the water generated in the reaction is continuously distilled out using an azeotropic agent; the alkali metal amide method uses an inert solvent such as toluene or heptane as the solvent for the reaction system, and alcohol reacts with alkali metal amide to prepare alcohol alkali metal salt; there is also a method of reacting low-carbon alcohol alkali metal salt with high-carbon alcohol to generate high-carbon alcohol alkali metal salt for preparing high-carbon alcohol alkoxide; in addition, there are methods such as the electrolysis method.

[0004] Among these methods, the metal method is unsafe, has high costs, large steam consumption, the alkali method has low content, high free alkali and low yield, the alkali metal amide method has expensive raw materials, the alcohol exchange method has high equipment and maintenance investment costs, and some of the other methods have imperfect routes, some have complex processes, or are expensive. Summary of the Invention

[0005] Aiming at the deficiencies existing in the prior art, the purpose of the utility model is to provide a synthesis device for medium-carbon alcohol alkoxide to solve the technical problem of high free alkali in the medium-carbon alcohol alkoxide synthesized by the existing synthesis device.

[0006] To solve the above technical problems, the utility model is realized by adopting the following technical solutions:

[0007] A synthesis device includes a reaction kettle, the reaction kettle is connected to the shell-side input end of a condenser, and the shell-side output end of the condenser is connected to a solvent receiving tank through a solvent recovery pump.

[0008] A reaction kettle jacket coil is further arranged outside the reaction kettle, and the reaction kettle jacket coil is connected to a cooling and heating circulation integrated machine.

[0009] The solid feed port of the reaction kettle is connected to a solid raw material storage tank through a scraper-type solid conveyor.

[0010] The liquid raw material inlet of the described reactor is connected to the liquid raw material dropping tank through a peristaltic pump.

[0011] The solvent inlet of the described reactor is connected to the solvent tank through a solvent material transfer pump.

[0012] The present utility model also has the following technical features:

[0013] A stirring paddle and a stirring motor are arranged inside the described reactor, and the stirring paddle is driven by the stirring motor.

[0014] A thermometer is arranged inside the described reactor.

[0015] The described reactor is provided with a protective gas inlet, and the described reactor is also connected to an exhaust safety valve through a condenser.

[0016] The discharging port of the described reactor is connected to the product receiving tank through a product material transfer pump.

[0017] Compared with the prior art, the present utility model has the following beneficial technical effects:

[0018] (Ⅰ) The free base obtained by the device of the present utility model is low, the solvent can be recycled and reused, and the product is easy to store.

[0019] (Ⅱ) The device combination of the present utility model is reasonable and the equipment requirements are low.

[0020] (Ⅲ) When the device of the present utility model prepares the product, the process is simple, the reaction process is carried out under mild conditions of normal pressure, and the reaction time is short. Description of the Drawings

[0021] Figure 1 It is a schematic structural diagram of a synthesis device for medium-carbon alcohol alkoxide.

[0022] The meanings of each label in the figure are as follows: 1 - reactor; 2 - condenser; 3 - solvent receiving tank; 4 - reactor jacket coil; 5 - cooling and heating circulation integrated machine; 6 - solid inlet; 7 - scraper type solid conveyor; 8 - solid raw material storage tank; 9 - liquid raw material inlet; 10 - peristaltic pump; 11 - liquid raw material dropping tank; 12 - solvent inlet; 13 - solvent material transfer pump; 14 - solvent tank; 15 - stirring paddle; 16 - stirring motor; 17 - thermometer; 18 - protective gas inlet; 19 - exhaust safety valve; 20 - discharging port; 21 - product material transfer pump; 22 - product receiving tank; 23 - pipeline; 24 - valve, 25 - solvent recovery pump.

[0023] The following further explains the specific content of the present utility model in detail in combination with embodiments. Detailed Embodiment

[0024] It should be noted that all the equipment and raw materials in the present invention, unless otherwise specified, are all equipment and raw materials known in the prior art.

[0025] In the utility model, various devices are connected mainly through pipelines 23, and valves 24 are provided on each pipeline as required, and are opened or closed according to process requirements.

[0026] All valves 24 in the present invention are valves commonly used in the prior art.

[0027] The medium-carbon alcohol in the present invention generally refers to a monohydric alcohol containing one hydroxyl group and having a molecular formula of 5 to 9 carbon atoms. The medium-carbon alcohol alkoxide is an alkali metal alkoxide synthesized using the medium-carbon alcohol as a raw material, mainly a sodium salt or a potassium salt.

[0028] The aliphatic hydrocarbon or aromatic hydrocarbon in the utility model is an inert hydrocarbon solvent.

[0029] The alkali metal hydride in the utility model mainly refers to sodium hydride or potassium hydride, both of which have a content of about 30wt.% and are sealed and preserved in mineral oil.

[0030] In accordance with the above technical solution, specific embodiments of the present utility model are given below. It should be noted that the present utility model is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solution of this application fall within the protection scope of the present utility model.

[0031] Embodiment 1:

[0032] This embodiment provides a synthesis device for a medium-carbon alcohol alkoxide, such as Figure 1 As shown, it includes a reactor 1, characterized in that the reactor 1 is connected to the shell side input end of the condenser 2, and the shell side output end of the condenser 2 is connected to the solvent receiving tank 3 through a solvent recovery pump 25.

[0033] like Figure 1 As shown, a reactor jacket coil 4 is also provided outside the reactor 1 , and the reactor jacket coil 4 is connected to a cooling and heating circulation integrated machine 5 .

[0034] like Figure 1 As shown, the solid feed port 6 of the reactor 1 is connected to the solid raw material storage tank 8 through a scraper-type solid conveyor 7 .

[0035] like Figure 1 As shown, the liquid raw material feed port 9 of the reactor 1 is connected to the liquid raw material dripping tank 11 through a peristaltic pump 10 .

[0036] like Figure 1 As shown, the solvent feed port 12 of the reaction kettle 1 is connected to the solvent tank 14 through a solvent material delivery pump 13 .

[0037] In this embodiment, the reaction kettle 1 is an enamel reaction kettle resistant to strong alkali and high temperature.

[0038] As a further solution of this embodiment, as Figure 1 shown, a stirring paddle 15 is arranged in the reaction kettle 1, and the stirring paddle 15 is driven by a stirring motor 16. Further preferably, the stirring paddle 15 adopts a six-inclined-blade turbine stirrer.

[0039] As a further solution of this embodiment, as Figure 1 shown, the reaction kettle 1 is provided with a thermometer 17, and the thermometer 17 displays the internal temperature of the reaction kettle in real time.

[0040] As a preferred solution of this embodiment, as Figure 1 shown, the reaction kettle 1 is provided with a protective gas inlet 18; the reaction kettle 1 is also connected to an exhaust safety valve 19 through a condenser 2.

[0041] As a preferred solution of this embodiment, as Figure 1 shown, the discharge port 20 of the reaction kettle 1 is connected to a product receiving tank 22 through a product material transfer pump 21.

[0042] The following takes the production of potassium tert-amylate as an example to illustrate the working process of the synthesis device for medium-carbon alcohol alkoxide:

[0043] The reaction kettle 1 is kept dry, nitrogen protection is turned on, and nitrogen is allowed to enter the reaction kettle 1 from the protective gas inlet 18. When feeding materials, the feeding valve 24 and the solvent material transfer pump 13 are opened, and 100 kg of cyclohexane in the solvent tank 14 is transported to the solvent feeding port 12 of the reaction kettle 1 for feeding; 20.7 kg of anhydrous potassium hydride in the solid raw material storage tank 8 is transported to the solid feeding port 6 of the reaction kettle 1 through a scraper-type solid conveyor 7 for feeding. The stirring motor 16 is turned on, and stirring is started using the stirring paddle 15, and the stirring speed is kept at 500 - 1000 rpm. The reaction kettle jacket coil 4 is heated, and the thermometer 17 is used for real-time detection until the reaction system reaches about 80 °C. 8.8 kg of tert-amyl alcohol in the liquid raw material dropping tank 11 is quantitatively and uniformly added dropwise to the liquid raw material feeding port 9 of the reaction kettle 1 using a peristaltic pump 10, and it is dropped in about 1 h. After the dropping is completed, the reaction continues until no more bubbles are generated, and then the reaction stops after 1 h; the reaction solution is distilled to obtain the target product potassium tert-amylate, and the distilled cyclohexane solvent enters the solvent receiving tank 3 after being condensed by the condenser 2 for recycling. After the reaction is completed, the nitrogen is discharged from the exhaust safety valve 19 behind the condenser 2. The discharge port 20 directly below the reaction kettle 1 is opened for discharging, and the discharged white potassium tert-amylate powder is transported to the product receiving tank 22 through the product material transfer pump 21 and the pipeline 23.

[0044] The obtained target product is 12.04 kg of off-white potassium tert-amylate powder, with a content of 99.7%, a free base of 0.2%, and a yield of 95.1%.

[0045] Elemental analysis: C, 47.55; H, 8.71; K, 30.99; O, 12.75

[0046] Product detection method:

[0047] (1) Determination of total alkali (content): Weigh about 0.5 g of the sample (accurate to 0.0002 g) and place it in a dry 100 mL iodine flask. Add about 20 mL of distilled water (boiled and cooled) to dissolve, shake well and let stand for 5 min. Add 3 drops of 1% phenolphthalein indicator, and titrate with 0.5 mol / L hydrochloric acid standard solution until it turns colorless as the end point. The total alkali content of potassium tert-butoxide is expressed as a mass fraction and calculated according to the following formula: X1 = C * V * 0.12624 / m * 100%, where: C represents the concentration of the hydrochloric acid standard solution (mol / L); V represents the volume of the hydrochloric acid standard solution consumed (mL); m represents the mass of the sample (g).

[0048] (2) Determination of free alkali:

[0049] Add 5 mL of benzoic acid - methanol solution and 15 - 20 mL of methanol as the mother liquor into the reaction flask, just covering the electrode. Titrate with Karl Fischer reagent until the pointer of the ammeter deflects greatly and remains unchanged for 30 s as the end point, without counting the consumption. Then weigh about 0.5 g of the sample (accurate to 0.0002 g), quickly add it into the reaction flask, and titrate with Karl Fischer reagent until the pointer of the ammeter deflects as much as in the blank experiment and remains unchanged for 30 s, which is the end point. Record the volume of Karl Fischer reagent consumed. The mass percentage of water is calculated according to the following formula: X2 = T * V / m * 100%. Where, T represents the titration degree of Karl Fischer reagent to water (g / mL); V represents the volume of Karl Fischer reagent consumed for titrating the sample (mL); m represents the mass of the sample (g). Take the arithmetic mean of the results of two parallel determinations as the determination result, and the difference between the results of two parallel determinations is not more than 0.1%. Then calculate the free alkali content according to the formula X3 = 3.111X2, where 3.111 is the conversion coefficient for converting water to potassium hydroxide.

[0050] Example 2:

[0051] This example gives a method for preparing a solution of potassium tert-hexoxide in heptane using the synthesis device of medium-carbon alcohol alkoxide given in Example 1.

[0052] The feeding method is the same as that in Example 1. The solvent is 120 kg of dry heptane, 19.5 kg of anhydrous potassium hydride. The heating jacket of the reaction kettle is turned on to heat up the reaction system to about 100 °C. 10.2 kg of tert-hexyl alcohol is added dropwise to the reaction solution, and it is added dropwise in about 1.5 h. After the addition is completed, the reaction continues for 5 h, and HPLC or GC is used for tracking detection. The detection method is to take a little reaction solution and dry it with a rotary evaporator. The reacted solution is detected to have no residual tert-hexyl alcohol, indicating that the reaction is completed. After the reaction is completed, the filtrate is prepared into a potassium tert-hexoxide heptane solution with a concentration of 9.71% for standby.

Claims

1. A synthesis device, comprising a reaction vessel (1), characterized in that: The reaction kettle (1) is connected to the shell side input end of the condenser (2), and the shell side output end of the condenser (2) is connected to the solvent receiving tank (3) through a solvent recovery pump (25); A reactor jacket coil (4) is also provided outside the reactor (1), and the reactor jacket coil (4) is connected to a cooling and heating circulation integrated machine (5); The solid feed port (6) of the reactor (1) is connected to the solid raw material storage tank (8) via a scraper-type solid conveyor (7); The liquid raw material feed port (9) of the reaction kettle (1) is connected to the liquid raw material dropping tank (11) via a peristaltic pump (10); The solvent feed port (12) of the reaction kettle (1) is connected to the solvent tank (14) via a solvent material delivery pump (13).

2. The synthesis device according to claim 1, characterized in that The reactor (1) is provided with a stirring paddle (15), and the stirring paddle (15) is driven by a stirring motor (16).

3. The synthesis device according to claim 1, characterized in that A thermometer (17) is arranged in the reaction kettle (1).

4. The synthesis device according to claim 1, characterized in that The reactor (1) is provided with a protective gas inlet (18); the reactor (1) is also connected to an exhaust safety valve (19) through the shell side of the condenser (2).

5. The synthesis device according to claim 1, characterized in that The discharge port (20) of the reaction kettle (1) is connected to the product receiving tank (22) via a product material delivery pump (21).

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