Organic phase and inorganic phase separation device in production of 2, 5-dimethyl-2, 5-hexanediol

Abstract

The utility model discloses an organic phase and inorganic phase separation device in 2, 5-dimethyl-2, 5-hexanediol production, which belongs to the field of chemical production devices and comprises an alkali liquor settling tank (1), a stop valve (6), an oil phase pump (7), a flow meter (24), a regulating valve (8), a jet type gas-liquid mixer (9) and a saline water separation tank (10) which are sequentially connected through pipelines. The discharge hole of the alkali liquor settling tank (1) is also sequentially connected with a conductivity (2), a stop valve (3), an alkali liquor pump (4), an alkali liquor tank (5), a conductivity (17), a stop valve (18), an alkali liquor pump (19), a stop valve (20), an alkali steaming kettle (22) and a byproduct alkali liquor tank (23) through pipelines; according to the utility model, the purposes of stable product quality, improved main content, and reduction of site exposure time and operation difficulty of personnel in a dangerous place can be achieved, and meanwhile, the safety risk and material waste caused by the fact that organic phases are discharged into the lye tank are avoided.

Description

Technical Field

[0001] The utility model relates to the field of chemical production equipment, in particular to an organic phase and inorganic phase separation device in the production of 2,5-dimethyl-2,5-hexanediol. Background Art

[0002] The general steps for producing 2,5-dimethyl-3-hexyne-2,5-diol are as follows: using a benzene series solvent and potassium hydroxide as a catalyst, acetylene and acetone are subjected to an acetylation reaction at normal pressure and a certain temperature to produce hexyne diol, followed by a catalytic hydrogenation reaction. The product is then separated by alkali solution, the oil phase is neutralized with an inorganic acid, the solvent is evaporated and recovered, dissolved in water, concentrated, centrifuged, and vaporized to obtain the product.

[0003] Among them, in the above production, there are generally two methods for separating the organic phase and the alkali solution: 1. Install a quartz glass tube sight glass on the alkali discharge pipe, and stop the discharge after the organic phase reaches the sight glass during manual continuous observation. This manual continuous observation is prone to fatigue, causing the organic phase to enter the alkali solution tank, resulting in increased raw material consumption and increased safety risks; 2. Use the method of Chinese patent application CN 115228144 A, that is, use a camera, host, controller, N-type tube and other equipment to automatically complete the alkali solution separation. This method is costly and unreliable, and is difficult to implement in industrial production.

[0004] The function of the neutralization device is to first separate the organic phase and the alkali solution, and then neutralize the trace potassium hydroxide in the organic phase. The existing neutralization device, whether described in CN 115090247 B or in actual production, adopts a batch production method of a kettle reactor. For the potassium chloride, potassium sulfate and potassium bicarbonate particles produced by the neutralization reaction according to the added inorganic acid, the particles are discharged by manual continuous observation through a quartz glass tube sight glass. The discharge is stopped when the organic phase reaches the sight glass. Manual continuous observation is prone to fatigue. If the organic phase reaches the sight glass in time, it is not detected, resulting in a large amount of oil phase entering the alkali solution tank, resulting in increased raw material consumption and increased safety risks. Summary of the Invention

[0005] The purpose of this utility model is to provide a device for separating the organic phase and the inorganic phase in the production of 2,5-dimethyl-2,5-hexanediol to solve the above problems.

[0006] In order to achieve the above-mentioned object, the technical solution adopted by the utility model is as follows: an organic phase and inorganic phase separation device for the production of 2,5-dimethyl-2,5-hexanediol comprises an alkali solution sedimentation tank, a shut-off valve B, an oil phase pump A, a flow meter A, a regulating valve A, a jet gas-liquid mixer and a brine separation tank connected in sequence through pipelines; the discharge port of the alkali solution sedimentation tank is also connected in sequence through pipelines to a conductivity meter A, a shut-off valve A, an alkali solution pump A, an alkali solution tank, an electrical conductivity meter B, a shut-off valve G, an alkali solution pump B, a shut-off valve H, an alkali steamer and a by-product alkali solution tank; the top of the jet gas-liquid mixer is also provided with a carbon dioxide inlet, and the pipeline is provided with a regulating valve B, a flow meter B and a shut-off valve C.

[0007] As a preferred technical solution: the discharge port of the brine separation tank is also connected to the alkali solution sedimentation tank, and a shut-off valve F is provided on the pipeline.

[0008] When the brine concentration in the brine separation tank reaches the control index, it will all be transferred to the alkali solution sedimentation tank. The brine separation tank here does not need to set the conductivity separately, and at the same time ensures that there are no errors in brine sampling and analysis. If the brine concentration is low, it can also be guaranteed to mix with the alkali solution in the alkali solution sedimentation tank to increase the concentration and reduce the concentration of organic matter it contains.

[0009] As a preferred technical solution: the discharge port of the alkali liquid tank is also connected to the alkali liquid sedimentation tank, and a shut-off valve I is provided on the pipeline.

[0010] The present application utilizes the difference in electrical conductivity between alkali solution, potassium chloride solution, potassium sulfate solution and potassium bicarbonate solution and the organic phase. When separating the above solutions, an online conductivity meter is used to continuously monitor and identify the conductivity, and then the signal is transmitted to the control room via an electrical signal to realize an automated cutting operation, thereby effectively separating the above solutions from the oil phase.

[0011] The organic phase is added with carbon dioxide through an oil phase pump and a jet gas-liquid mixer and continuously enters a brine separation tank with a fixed volume of recycled water. The amount of carbon dioxide added is controlled by the flow rate of the oil phase pump. The final pressure of the brine separation tank is 0.03MPa and maintained for 15 minutes as the end time of the reaction. After each batch of neutralization is completed, the total concentration of potassium carbonate and potassium bicarbonate in the brine is analyzed. If the total concentration exceeds 21%, the brine needs to be transferred to an alkali solution separation tank and new return water is added to the brine separation tank. This method reduces the number of neutralization kettles and realizes continuous automated operation, reduces the amount of potassium carbonate and potassium bicarbonate in the organic phase, reduces the time of personnel exposure on site, and makes the pH value of the acetylene water more stable.

[0012] Compared with the existing technology, the advantages of the present invention are: the separation device of the present invention can achieve the purpose of stable product quality, improved main content, reduced on-site exposure time of personnel in dangerous places and operation difficulty, while avoiding the discharge of organic phase into the alkali solution tank to form safety risks and material waste. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 This is a structural diagram of Example 1 of the present utility model;

[0014] In the figure, 1. alkali solution settling tank; 2. conductivity meter A; 3. shut-off valve A; 4. alkali solution pump A; 5. alkali solution tank; 6. shut-off valve B; 7. oil phase pump A; 8. regulating valve A; 9. jet gas-liquid mixer; 10. brine separation tank; 11. shut-off valve C; 12. regulating valve B; 13. shut-off valve D; 14. oil phase pump B; 15. shut-off valve E; 16. shut-off valve F; 17. conductivity meter B; 18. shut-off valve G; 19. alkali solution pump B; 20. shut-off valve H; 21. shut-off valve I; 22. alkali still; 23. by-product alkali solution tank; 24. flow meter A; 25. flow meter B. DETAILED DESCRIPTION

[0015] The present invention will be further described below with reference to the accompanying drawings. Example

[0016] See also Figure 1 , a device for separating organic and inorganic phases in the production of 2,5-dimethyl-2,5-hexanediol, comprising an alkali solution sedimentation tank 1, a shut-off valve B6, an oil phase pump A7, a flow meter A24, a regulating valve A8, a jet gas-liquid mixer 9, and a brine separation tank 10, which are sequentially connected through pipelines; the discharge port of the alkali solution sedimentation tank 1 is also sequentially connected to a conductivity meter A2, a shut-off valve A3, an alkali solution pump A4, an alkali solution tank 5, a conductivity meter B17, a shut-off valve G18, an alkali solution pump B19, a shut-off valve H20, an alkali steaming kettle 22, and a by-product alkali solution tank 23 through pipelines; a carbon dioxide inlet is also provided at the top of the jet gas-liquid mixer 9, and a regulating valve B12, a flow meter B25, and a shut-off valve C11 are provided on the pipeline;

[0017] In this embodiment: the discharge port of the brine separation tank 10 is also connected to the alkali solution sedimentation tank 1, and a cut-off valve F16 is provided on the pipeline;

[0018] The discharge port of the alkali solution tank 5 is also connected to the alkali solution sedimentation tank 1, and a shut-off valve I21 is also provided on the pipeline;

[0019] Figure 1 The direction of the arrow in the middle is the direction of material flow, among which arrow a is "material from acetylation reaction", arrow b is "carbon dioxide from storage tank", arrow c is "to tank truck", and arrow d is "to solvent recovery device".

[0020] Unless otherwise specified, the components of the above devices can be obtained commercially.

[0021] The functions of the above main equipment are:

[0022] Alkali liquid sedimentation tank 1: completes the sedimentation of organic phase and alkali liquid;

[0023] Conductivity meter A2, conductivity meter B17: measure the real-time conductivity of the liquid and convert the conductivity value into mA signal and transmit it to the host computer;

[0024] Jet-type gas-liquid mixer 9: used to complete the mixing and reaction of trace potassium hydroxide and carbon dioxide in the organic phase;

[0025] Brine separation tank 10: used for washing and sedimentation separation of suspended potassium carbonate and potassium bicarbonate particles in the organic phase;

[0026] Alkali liquid tank 5: used to store the alkali liquid separated by the alkali liquid sedimentation tank 1 and perform secondary sedimentation;

[0027] Alkali steaming kettle 22: used to distill out trace organic matter in the alkali solution in the alkali solution tank 5;

[0028] Byproduct lye tank 23: used to store the lye after distillation for sale.

[0029] A process using the above-mentioned device;

[0030] The materials from the acetylation reaction process were placed in an alkali solution settling tank 1. After settling for 4 hours, the shut-off valve A3 was opened and the alkali solution pump A4 was started to transfer the lower alkali solution into the alkali solution tank 5. When the value measured by the conductivity meter A2 was less than 100 μs / cm, the shut-off valve A3 was closed and the alkali solution pump A4 was stopped to complete the separation of the organic phase and the alkali solution.

[0031] Neutralization of organic phase: first add 500L of production water to the brine separation tank 10, then open the shut-off valve C11, adjust the regulating valve B12, and keep the flow meter B25 display at 30m 3 / h; then open the shut-off valve B6, start the oil phase pump A7, and adjust the regulating valve A8 so that the flow meter A24 displays at 15m 3 / h, when the material in the alkali solution settling tank 1 is transferred, close the shut-off valve B6, stop the oil phase pump A7, close the regulating valve A8 and continue to introduce carbon dioxide gas. When the pressure of the brine separation tank 10 reaches 50kPa, stop adding carbon dioxide gas and maintain the pressure at 50kPa. After 15 minutes, vent and complete neutralization. After settling for 2 hours, open the shut-off valve D13 and the shut-off valve E15 to start the oil phase pump B14 to transfer the organic phase to the solvent recovery device. After 3 batches, take the lower water sample from each batch and stratify the potassium carbonate and potassium bicarbonate concentrations. When the concentration is greater than 28wt%, open the shut-off valve D13 and the shut-off valve F16 to start the oil phase pump B14 to transfer the lower brine to the alkali solution settling tank 1;

[0032] After secondary sedimentation in the alkali liquid tank 5, the alkali liquid is transferred to the alkali steam kettle 22 through the conductivity meter B17, the shut-off valve G18, the alkali liquid pump B19, and the shut-off valve H20. The alkali liquid is distilled under reduced pressure to the boiling temperature and maintained for 30 minutes before being placed in the by-product alkali liquid tank 23 for storage. When the alkali liquid is transferred to the alkali steam kettle 22, when the value measured by the conductivity meter B17 is less than 100μs / cm, the shut-off valve H20 is closed and the alkali liquid pump B19 is stopped. After verifying the production status of the alkali liquid sedimentation tank 1, the shut-off valve I21 is opened and the alkali liquid pump B19 is started to transfer all the upper organic phase of the alkali liquid tank 5 to the alkali liquid sedimentation tank 1.

[0033] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A device for separating organic and inorganic phases in the production of 2,5-dimethyl-2,5-hexanediol, characterized in that: The invention comprises an alkali solution settling tank (1), a shut-off valve B (6), an oil phase pump A (7), a flow meter A (24), a regulating valve A (8), a jet gas-liquid mixer (9) and a brine separation tank (10) which are connected in sequence through pipelines; the discharge port of the alkali solution settling tank (1) is further connected in sequence through pipelines to a conductivity meter A (2), a shut-off valve A (3), an alkali solution pump A (4), an alkali solution tank (5), an electrical conductivity meter B (17), a shut-off valve G (18), an alkali solution pump B (19), a shut-off valve H (20), an alkali steaming kettle (22) and a by-product alkali solution tank (23); a carbon dioxide inlet is further provided at the top of the jet gas-liquid mixer (9), and a regulating valve B (12), a flow meter B (25) and a shut-off valve C (11) are provided on the pipeline.

2. The device for separating organic and inorganic phases in the production of 2,5-dimethyl-2,5-hexanediol according to claim 1, characterized in that: The discharge port of the brine separation tank (10) is also connected to the alkali solution sedimentation tank (1), and a shut-off valve F (16) is provided on the pipeline.

3. The device for separating organic and inorganic phases in the production of 2,5-dimethyl-2,5-hexanediol according to claim 1, characterized in that: The discharge port of the alkali solution tank (5) is also connected to the alkali solution sedimentation tank (1), and a shut-off valve I (21) is provided on the pipeline.

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