A preparation process for high-purity and high-yield acetylene glycol

Abstract

The present invention discloses a process for preparing high-purity and high-yield acetylene glycol, and relates to the technical field of surfactants. The process for preparing high-purity and high-yield acetylene glycol in the present invention comprises a synthesis reaction, water washing, standing, low-temperature water washing, secondary standing, and distillation. The water washing removes a small amount of potassium hydroxide and raw material ketone remaining in the system. After standing at room temperature, an organic phase is separated by separation. The temperature is then lowered and low-temperature water washing is performed to remove the raw material ketone slightly soluble in water. After two consecutive water washing and standing conditions with different temperatures, the impurities of the acetylene glycol in the organic phase are only a small amount of raw material ketone and solvent methyl tert-butyl ether. During distillation, the temperature is increased and a large amount of water is added as an azeotropic agent to perform distillation and desolvation. The methyl tert-butyl ether is first completely distilled off, and then the water and raw material ketone are distilled off, thereby obtaining high-purity and high-yield acetylene glycol.

Description

Technical Field

[0001] The invention relates to the technical field of surfactants, and in particular to a preparation process of high-purity and high-yield acetylene glycol. Background Art

[0002] Commonly used alkynol compounds today include propynol, methylbutynol, methylpentynol, hexynol, 3,6-dimethyl-4-octyne-3,6-diol, 2,5-dimethyl-3-hexyne-2,5-diol, ethyloctyne alcohol, etc. These alkynols have different physical properties but similar structures. In addition to the alkynyl group, they all contain polar group hydroxyl and polar group hydrocarbon group. This structure determines that alkynol compounds have many excellent properties.

[0003] Acetylene glycol surfactants are nonionic surfactants in water-based systems that significantly reduce the surface tension of water. These multifunctional surfactants are often compounded with various solvents to form liquids for ease of use. They are widely used in water-based coatings, dyes, inks, pesticides, and other fields. They can be used as wetting agents and defoamers in water-based coatings, improving coating uniformity and flowability, and exhibit excellent performance.

[0004] Currently, the main industrial synthesis methods for alkynols include: solid potassium hydroxide catalytic acetylation, catalytic acetylation in the presence of liquid ammonia and potassium hydroxide, and potassium alcoholate catalytic acetylation. The catalytic acetylation in the presence of liquid ammonia and potassium hydroxide has the following disadvantages: the high volatility of liquid ammonia requires pressurization, which requires a large equipment investment, and the use of pressurized acetylene requires special safety measures to ensure safety. These synthesis methods not only have some disadvantages, but also the purity and yield of the decynediol produced are not high. Therefore, the present invention studies a preparation process for high-purity, high-yield acetylenic diol. Summary of the Invention

[0005] The object of the present invention is to provide a process for preparing high-purity and high-yield acetylene glycol to solve the problems raised in the above background technology.

[0006] In order to solve the above technical problems, the present invention provides the following technical solution: a preparation process of high-purity and high-yield acetylene glycol, wherein the preparation process of high-purity and high-yield acetylene glycol comprises a synthesis reaction, water washing, standing, low-temperature water washing, secondary standing and distillation.

[0007] Preferably, the raw materials for preparing acetylene diol in the high-purity and high-yield acetylene diol preparation process are ketone, acetylene and catalyst; the molar ratio of ketone, acetylene and catalyst is 1:0.5-2:1.1-2.5; and the ketone is one of methyl isobutyl ketone or methyl isoamyl ketone.

[0008] Preferably, the catalyst is potassium hydroxide in a mass fraction.

[0009] Preferably, the low-temperature water washing is performed at a temperature of -2 to 2°C.

[0010] Preferably, an entrainer is added during the distillation; the entrainer is water.

[0011] Preferably, a process for preparing high-purity and high-yield acetylene glycol comprises the following specific steps:

[0012] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and the catalyst into the reactor, mix and stir evenly, raise the temperature to 20-40°C under normal pressure, introduce ketone and acetylene, and react for 2-4 hours;

[0013] (2) Water washing: washing the product obtained in step (1) with water for 1 to 2 hours; separating the organic phase;

[0014] (3) Standing: The organic phase obtained in step (2) is allowed to stand for 1 to 3 hours;

[0015] (4) Low-temperature water washing: The liquid after step (3) is washed with low-temperature water for 1 to 3 hours at a temperature of -2 to 2°C.

[0016] (5) Second standing: time is 30-90 min, temperature is 0-2°C, and crude acetylenediol is separated;

[0017] (6) Distillation: Add an azeotropic agent and raise the temperature to 60-80°C. Distill for 20-30 minutes, then raise the temperature to 110-130°C again and distill for 1-3 hours.

[0018] Preferably, in the above step (1), the mass ratio of methyl tert-butyl ether to catalyst is 2.1-2.5:0.04-0.06.

[0019] Preferably, in the above step (1), the ventilation time of ketone is 5 to 8 hours.

[0020] Preferably, in the above step (1), the ventilation time of acetylene is 6 to 9 hours.

[0021] Preferably, in the above step (6), the mass ratio of the entrainer to methyl tert-butyl ether is 1.6 to 1.8:1.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] The preparation process of high-purity and high-yield acetylene glycol of the present invention comprises synthesis reaction, water washing, standing, low-temperature water washing, secondary standing and distillation.

[0024] During water washing, a small amount of potassium hydroxide and raw material ketone remaining in the system is removed. After standing at room temperature, an organic phase is separated by stratification. The temperature is then lowered for low-temperature water washing to remove the raw material ketone slightly soluble in water again. After two consecutive water washing and standing environments with temperature differences, the impurities of the acetylene glycol in the organic phase are only a small amount of raw material ketone and solvent methyl tert-butyl ether. During distillation, the temperature is increased and a large amount of water is added as an azeotropic agent to perform distillation and desolvation. The methyl tert-butyl ether is first completely distilled out, and then the water and the raw material ketone are distilled out to obtain high-purity and high-yield acetylene glycol. DETAILED DESCRIPTION

[0025] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0026] Example 1

[0027] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.1:0.04, mix and stir evenly, raise the temperature to 20°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:0.5:1.1, the ventilation time of methyl isobutyl ketone is 5 hours, the reaction time is 2 hours, and the ventilation time of acetylene is 6 hours;

[0028] (2) Water washing: washing the product obtained in step (1) with water for 1 h; separating the organic phase;

[0029] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 1 h;

[0030] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 1 hour at a temperature of -2°C;

[0031] (5) Second standing: time is 30 min, temperature is 0°C, and crude decynediol is separated;

[0032] (6) Distillation: Add an entrainer and raise the temperature to 60°C. Distill for 20 minutes, then raise the temperature to 110°C and distill for 1 hour. The mass ratio of entrainer to methyl tert-butyl ether is 1.6:1. The purity of decynediol is ≥99%, and the yield is 92.8%.

[0033] Example 2

[0034] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.3:0.05, mix and stir evenly, raise the temperature to 30°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:1.25:1.8, the ventilation time of methyl isobutyl ketone is 6 hours, the reaction time is 3 hours, and the ventilation time of acetylene is 8 hours;

[0035] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0036] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0037] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0038] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0039] (6) Distillation: Add an entrainer and raise the temperature to 70°C. Distill for 25 minutes, then raise the temperature to 120°C and distill for 2 hours. The mass ratio of entrainer to MTBE is 1.7:1. The purity of decynediol is ≥99%, and the yield is 93.6%.

[0040] Example 3

[0041] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.5:0.06, mix and stir evenly, heat to 40°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:2:2.5, the ventilation time of methyl isobutyl ketone is 8 hours, the ventilation time of acetylene is 9 hours, and the reaction is carried out for 4 hours;

[0042] (2) Water washing: The product obtained in step (1) was washed with water for 2 h; and the organic phase was separated;

[0043] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 3 h;

[0044] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 3 hours at a temperature of 2°C;

[0045] (5) Second standing: time: 90 min, temperature: 2°C, to separate crude decynediol;

[0046] (6) Distillation: Add an entrainer and raise the temperature to 80°C. Distill for 30 minutes, then raise the temperature to 130°C and distill for 3 hours. The mass ratio of entrainer to MTBE is 1.8:1. The purity of decynediol is ≥99%, and the yield is 92.2%.

[0047] Example 4

[0048] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and potassium hydroxide (catalyst) were added to the reactor in a mass ratio of 2.1:0.04, mixed and stirred evenly, and then heated to 20°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced in a molar ratio of methyl isoamyl ketone, acetylene, and catalyst of 1:0.5:1.1. The methyl isoamyl ketone was aerated for 5 h, the reaction was allowed to proceed for 2 h, and the acetylene was aerated for 6 h.

[0049] (2) Water washing: washing the product obtained in step (1) with water for 1 h; separating the organic phase;

[0050] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 1 h;

[0051] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 1 hour at a temperature of -2°C;

[0052] (5) Second standing: time is 30 min, temperature is 0°C, and crude decynediol is separated;

[0053] (6) Distillation: Add an entrainer and raise the temperature to 60°C. Distill for 20 minutes, then raise the temperature to 110°C and distill for 1 hour. The mass ratio of entrainer to methyl tert-butyl ether is 1.6:1. The purity of dodecynediol is ≥99%, and the yield is 93.8%.

[0054] Example 5

[0055] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.3:0.05, mixed and stirred evenly, and the temperature was raised to 30°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced. The molar ratio of methyl isoamyl ketone, acetylene and catalyst was 1:1.25:1.8. The ventilation time of methyl isoamyl ketone was 6 hours, the reaction was carried out for 3 hours, and the ventilation time of acetylene was 8 hours.

[0056] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0057] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0058] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0059] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0060] (6) Distillation: Add an entrainer and raise the temperature to 70°C. Distill for 25 minutes, then raise the temperature to 120°C and distill for 2 hours. The mass ratio of entrainer to methyl tert-butyl ether is 1.7:1. The purity of dodecynediol is ≥99%, and the yield is 93.4%.

[0061] Example 6

[0062] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.5:0.06, mixed and stirred evenly, and the temperature was raised to 40°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced into the reactor in a molar ratio of methyl isoamyl ketone, acetylene, and catalyst of 1:2:2.5. The ventilation time of methyl isoamyl ketone was 8 hours, the ventilation time of acetylene was 9 hours, and the reaction was carried out for 4 hours.

[0063] (2) Water washing: The product obtained in step (1) was washed with water for 2 h; and the organic phase was separated;

[0064] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 3 h;

[0065] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 3 hours at a temperature of 2°C;

[0066] (5) Second standing: time: 90 min, temperature: 2°C, to separate crude decynediol;

[0067] (6) Distillation: Add an entrainer and raise the temperature to 80°C. Distill for 30 minutes, then raise the temperature to 130°C and distill for 3 hours. The mass ratio of entrainer to MTBE is 1.8:1. The purity of dodecanediol is ≥99%, and the yield is 93.2%.

[0068] Comparative Example 1

[0069] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.3:0.05, mix and stir evenly, raise the temperature to 30°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:1.25:1.8, the ventilation time of methyl isobutyl ketone is 6 hours, the reaction time is 3 hours, and the ventilation time of acetylene is 8 hours;

[0070] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0071] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0072] (4) Distillation: Add an entrainer and raise the temperature to 70°C. Distill for 25 minutes, then raise the temperature to 120°C and distill for 2 hours. The mass ratio of entrainer to MTBE is 1.7:1. The purity of decynediol is 98.3%, and the yield is 88.3%.

[0073] Comparative Example 2

[0074] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.3:0.05, mix and stir evenly, raise the temperature to 30°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:1.25:1.8, the ventilation time of methyl isobutyl ketone is 6 hours, the reaction time is 3 hours, and the ventilation time of acetylene is 8 hours;

[0075] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0076] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0077] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0078] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0079] (6) Distillation: Add an entrainer and raise the temperature to 120°C. Distill for 2 hours. The mass ratio of entrainer to methyl tert-butyl ether is 1.7:1. The purity of decynediol is 98.1%, and the yield is 78.4%.

[0080] Comparative Example 3

[0081] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.3:0.05, mix and stir evenly, raise the temperature to 30°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:1.25:1.8, the ventilation time of methyl isobutyl ketone is 6 hours, the reaction time is 3 hours, and the ventilation time of acetylene is 8 hours;

[0082] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0083] (3) Standing: The organic phase obtained in step (2) is allowed to stand for 2 hours;

[0084] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0085] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0086] (6) Distillation: Heat to 120°C and distill for 2 hours. The purity of decynediol is 97.3%, and the yield is 75.9%.

[0087] Comparative Example 4

[0088] (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and catalyst potassium hydroxide into the reactor at a mass ratio of 2.3:0.05, mix and stir evenly, raise the temperature to 30°C under normal pressure, introduce methyl isobutyl ketone and acetylene, the molar ratio of methyl isobutyl ketone, acetylene and catalyst is 1:1.25:1.8, the ventilation time of methyl isobutyl ketone is 6 hours, the reaction time is 3 hours, and the ventilation time of acetylene is 8 hours;

[0089] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0090] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0091] (4) Distillation: Heat to 120°C and distill for 2 hours. The purity of decynediol is 94.6%, and the yield is 71.5%.

[0092] Comparative Example 5

[0093] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.3:0.05, mixed and stirred evenly, and the temperature was raised to 30°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced. The molar ratio of methyl isoamyl ketone, acetylene and catalyst was 1:1.25:1.8. The ventilation time of methyl isoamyl ketone was 6 hours, the reaction was carried out for 3 hours, and the ventilation time of acetylene was 8 hours.

[0094] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0095] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0096] (4) Distillation: Add an entrainer and raise the temperature to 70°C. Distill for 25 minutes, then raise the temperature to 120°C and distill for 2 hours. The mass ratio of entrainer to methyl tert-butyl ether is 1.7:1. The purity of dodecynediol is 98.7%, and the yield is 85.4%.

[0097] Comparative Example 6

[0098] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.3:0.05, mixed and stirred evenly, and the temperature was raised to 30°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced. The molar ratio of methyl isoamyl ketone, acetylene and catalyst was 1:1.25:1.8. The ventilation time of methyl isoamyl ketone was 6 hours, the reaction was carried out for 3 hours, and the ventilation time of acetylene was 8 hours.

[0099] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0100] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0101] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0102] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0103] (6) Distillation: Add an entrainer and raise the temperature to 120°C. Distill for 2 hours. The mass ratio of entrainer to methyl tert-butyl ether is 1.7:1. The purity of dodecynediol is 97.8%, and the yield is 79.4%.

[0104] Comparative Example 7

[0105] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.3:0.05, mixed and stirred evenly, and the temperature was raised to 30°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced. The molar ratio of methyl isoamyl ketone, acetylene and catalyst was 1:1.25:1.8. The ventilation time of methyl isoamyl ketone was 6 hours, the reaction was carried out for 3 hours, and the ventilation time of acetylene was 8 hours.

[0106] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0107] (3) Standing: The organic phase obtained in step (2) is allowed to stand for 2 hours;

[0108] (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 2 hours at a temperature of 0°C;

[0109] (5) Second standing: time: 60 min, temperature: 1°C, to separate the crude decynediol;

[0110] (6) Distillation: Heat to 120°C and distill for 2 hours. The purity of dodecynediol is 97.6%, and the yield is 75.1%.

[0111] Comparative Example 8

[0112] (1) Synthesis reaction: The air in the reactor was replaced with nitrogen, and methyl tert-butyl ether and the catalyst potassium hydroxide were added to the reactor in a mass ratio of 2.3:0.05, mixed and stirred evenly, and the temperature was raised to 30°C under normal pressure. Methyl isoamyl ketone and acetylene were introduced. The molar ratio of methyl isoamyl ketone, acetylene and catalyst was 1:1.25:1.8. The ventilation time of methyl isoamyl ketone was 6 hours, the reaction was carried out for 3 hours, and the ventilation time of acetylene was 8 hours.

[0113] (2) Water washing: The product obtained in step (1) was washed with water for 1.5 h; and the organic phase was separated;

[0114] (3) Standing: The organic phase obtained in step (2) was allowed to stand for 2 h;

[0115] (4) Distillation: Heat to 120°C and distill for 2 hours. The purity of dodecanediol is 95.1% and the yield is 72.4%.

[0116] Effect Examples

[0117] Table 1 below shows the performance analysis results of the acetylene glycols of Examples 1 to 6 of the present invention and Comparative Examples 1 to 8:

[0118] Table 1

[0119] purity(%) Yield (%) purity(%) Yield (%) Example 1 ≥99 92.8 Comparative Example 2 98.1 78.4 Example 2 ≥99 93.6 Comparative Example 3 97.3 75.9 Example 3 ≥99 92.2 Comparative Example 4 94.6 71.5 Example 4 ≥99 93.8 Comparative Example 5 98.7 85,4 Example 5 ≥99 93.4 Comparative Example 6 97.8 79.4 Example 6 ≥99 93.2 Comparative Example 7 97.6 75.1 Comparative Example 1 98.3 88.3 Comparative Example 8 95.1 72.4

[0120] By comparing the experimental data of the examples and the comparative examples in Table 1, it can be clearly found that the purity and yield of the acetylene glycols prepared in Examples 1-6 are higher.

[0121] From the comparison of the experimental data of Examples 1-6 and Comparative Examples 1, 4, 5 and 8, it can be found that after the first water washing and standing, the subsequent water washing and standing at lower temperatures can remove the raw ketones that are slightly soluble in water, reduce the impurities in the organic phase, and improve the purity;

[0122] From the comparison of the experimental data of Examples 1-6 and Comparative Examples 3, 4, 7 and 8, it can be found that during distillation, increasing the temperature and adding a large amount of water as an azeotropic agent for distillation and desolvation can reduce impurities and improve the purity and yield of the product;

[0123] From the comparison of the experimental data of Examples 1-6 and Comparative Examples 2, 4, 6 and 8, it can be found that by adding an azeotropic agent and performing distillation, adjusting the temperature to first distill off all the methyl tert-butyl ether, and then distilling off the water and the raw material ketone, high purity and high yield of acetylene glycol can be obtained.

[0124] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be encompassed therein. Any reference in a claim should not be construed as limiting the claim to which it relates.

Claims

1. A process for preparing high-purity and high-yield acetylene glycol, characterized in that: The preparation process of high-purity and high-yield acetylene glycol comprises a synthesis reaction, water washing, standing, low-temperature water washing, secondary standing and distillation; The specific steps include: (1) Synthesis reaction: replace the air in the reactor with nitrogen, add methyl tert-butyl ether and the catalyst into the reactor, mix and stir evenly, raise the temperature to 20-40°C under normal pressure, introduce ketone and acetylene, and react for 2-4 hours; (2) Water washing: washing the product obtained in step (1) with water for 1 to 2 hours; separating the organic phase; (3) Standing: The organic phase obtained in step (2) is allowed to stand for 1 to 3 hours; (4) Low-temperature water washing: The liquid after standing in step (3) is washed with low-temperature water for 1 to 3 hours at a temperature of -2 to 2°C; (5) Second standing: time is 30-90 min, temperature is 0-2°C, and crude acetylenediol is separated; (6) Distillation: Add an azeotropic agent and heat to 60-80°C, distill for 20-30 minutes, then heat again to 110-130°C and distill for 1-3 hours; In the above step (1), the mass ratio of methyl tert-butyl ether to catalyst is 2.1-2.5:0.04-0.

06.

2. A process for preparing high-purity and high-yield acetylenediol according to claim 1, characterized in that: The raw materials for preparing the acetylene glycol in the high-purity and high-yield acetylene glycol preparation process are ketone, acetylene and a catalyst; the molar ratio of the ketone, acetylene and catalyst is 1:0.5-2:1.1-2.5; and the ketone is one of methyl isobutyl ketone and methyl isoamyl ketone.

3. A process for preparing high-purity and high-yield acetylene glycol according to claim 1, characterized in that: The catalyst is potassium hydroxide.

4. A process for preparing high-purity and high-yield acetylene glycol according to claim 1, characterized in that: The entrainer is water.

5. A process for preparing high-purity and high-yield acetylene glycol according to claim 1, characterized in that: In the above step (1), the ventilation time of ketone is 5 to 8 hours.

6. A process for preparing high-purity and high-yield acetylene glycol according to claim 1, characterized in that: In the above step (1), the ventilation time of acetylene is 6 to 9 hours.

7. A process for preparing high-purity and high-yield acetylene glycol according to claim 1, characterized in that: In the above step (6), the mass ratio of the entrainer to methyl tert-butyl ether is 1.6 to 1.8:1.