Preparation device and method of alkynol compound

Abstract

The invention discloses a device and a method for preparing alkynol compounds. The device for preparing the alkynol compounds comprises a catalyst storage tank, a solvent storage tank, an acetylene storage tank, a ketone monomer storage tank, an emulsifier, a mixer and a reaction kettle, the catalyst storage tank and the solvent storage tank are communicated with the emulsifier; the acetylene storage tank and the ketone monomer storage tank are communicated with the mixer; a discharge hole of the reaction kettle is formed in the upper part of the reaction kettle, the emulsifier is communicated with the reaction kettle through a pipeline, a discharge hole of the pipeline is positioned in the middle of the reaction kettle, and the mixer is communicated with the bottom of the reaction kettle. According to the device provided by the invention, a mixture of acetylene and ketone is fed from the bottom of the reaction kettle, slurry obtained by homogenizing and emulsifying a catalyst and a solvent is fed from the middle of the reaction kettle, and meanwhile, a reaction product overflows from the upper part of the reaction kettle, so that positive pressure is kept in the reaction kettle, forward reaction is promoted, continuous production of alkynol compounds is realized, and the production cost is reduced. The reaction process is stable and controllable, the product purity is high, and the yield is high.

Description

Technical Field

[0001] The invention relates to the technical field of organic synthesis, and in particular to a device and a method for preparing alkynol compounds. Background Art

[0002] Alkynol products have excellent properties due to the triple bonds and hydroxyl active groups they contain. They are a type of excellent water-based nonionic surfactant that can significantly reduce the surface tension of water. They are usually compounded with various solvents to form liquids for easy use. Functional alkynol epoxy derivatives can be synthesized using alkynol and ethylene (propylene) oxide as raw materials; silicone-modified alkynol ethers can be synthesized using alkynol ethers and hydrogen-containing siloxanes as raw materials. They are widely used as wetting agents and defoamers for water-based coatings to improve the uniformity and fluidity of coatings. They can also be used in dyes, pesticides, and water-based inks. They are widely used. At the same time, decynediol can be synthesized for the interface control material used in photovoltaic silicon wafer cutting to solve the technical problems of obvious line marks, excessive TTV, broken wires, broken edges, high roughness and warpage in the current silicon wafer cutting process.

[0003] There are many literatures and related patent reports on the synthesis of alkynols, most of which use strong bases as catalysts. For example, the current domestic industrial production uses potassium hydroxide as a catalyst, ether, alkane or alkylbenzene as a solvent, and acetylene and ketone are reacted to produce it. Patent CN201610488196.2 applied for by Southwest Chemical Research and Design Institute Co., Ltd. mentions that ammonia is used as a solvent, and acetylene and ammonia are mixed and compressed. This method has great safety hazards. Patent CN201711365712.3 applied for by Wang Jianhua uses a potassium hydroxide complex as a catalyst, specifically potassium hydroxide / pod ether complex as a catalyst. Pod ether uses diethylene glycol divinyl ether to achieve the best effect. The use of this catalyst can greatly reduce the amount of catalyst used, but the complex catalyst is difficult to remove trace moisture after hydrolysis treatment, and moisture is not good for the acetylation reaction, and the ideal effect of reducing production costs cannot be achieved. Foreign Italian patents 590732, 650164, 778013, 684731, 692788, 695546, U.S. patents 3283014, 3301771, 4614600, 4670186, 4028268, etc., and British patents 902014, 93563, 938849, 1041052, 1023856, 938849, 0183353, etc. have also conducted relevant research on the production and application of alkynols.

[0004] However, the preparation of alkynol compounds in the prior art mostly adopts intermittent reactors, which have the problem of large amounts of solvent and potassium hydroxide, long reaction time, and the by-product potassium hydroxide solution cannot be reused after the product is hydrolyzed. Moreover, for the reaction in which acetylene participates under pressure, there are drawbacks such as high flammability and explosion hazard of acetylene, which is difficult to scale up safely. In addition, the current kettle production capacity is limited, and there is no report on the use of continuous flow process production. The greatest difficulty lies in the metering and transportation of potassium hydroxide solids, which makes it difficult to achieve its uniform and stable feeding. Summary of the invention

[0005] In view of the above-mentioned shortcomings, the object of the present invention is to provide a device and method for preparing acetylene alcohol compounds, so as to solve the technical problems that the existing acetylene alcohol compounds cannot achieve continuous production and the product yield is low.

[0006] To achieve the above object, the present invention is implemented through the following technical solutions: In a first aspect, the present invention provides a device for preparing acetylene alcohol compounds, comprising a catalyst storage tank, a solvent storage tank, an acetylene storage tank, a ketone monomer storage tank, an emulsifier, a mixer and a reactor; wherein the catalyst storage tank and the solvent storage tank are connected to the emulsifier, and the acetylene storage tank and the ketone monomer storage tank are connected to the mixer; the discharge port of the reactor is arranged at the upper part of the reactor, the emulsifier is connected to the reactor through a pipeline, and the discharge port of the pipeline is located in the middle part of the reactor, and the mixer is connected to the bottom of the reactor.

[0007] Preferably, the above-mentioned device also includes a first flow controller, a second flow controller, a third flow controller and a fourth flow controller; the first flow controller is arranged on the catalyst feed pipeline, the second flow controller is arranged on the solvent feed pipeline, the third flow controller is arranged on the acetylene feed pipeline, and the fourth flow controller is arranged on the ketone monomer feed pipeline.

[0008] Preferably, there are multiple reactors, and the multiple reactors are arranged in series through pipelines, and the discharge ports of the pipelines are located in the middle of the reactors.

[0009] Preferably, a stirring assembly is provided in the reactor; the reactor is a stainless steel reactor.

[0010] Preferably, the above device further comprises an aging hydrolysis kettle, which is connected to the discharge port of the reaction kettle.

[0011] In a second aspect, the present invention provides a method for preparing an alkynol compound, using the preparation device for the alkynol compound as described in the first aspect, and the preparation method comprises the following steps: Passing the catalyst and the solvent into an emulsifier for homogenization and emulsification to obtain an emulsified slurry; The acetylene and ketone monomers are introduced into a mixer and mixed evenly to obtain a mixture; The mixed material is fed from the bottom of the reactor, and the emulsified slurry is fed from the middle of the reactor, so that acetylene and ketone monomers are fully reacted in the reactor, and the acetylene alcohol compounds generated by the reaction and unreacted acetylene overflow from the upper part of the reactor.

[0012] Preferably, the molar ratio of the ketone monomer, acetylene and catalyst is 1:(0.5-1.5):(0.5-2), and the amount of the solvent used is 2-5 times the mass of the catalyst.

[0013] Preferably, the catalyst is a strong base, and the solvent is at least one of an ether compound, an alkane compound, and a benzene compound.

[0014] Preferably, the reaction temperature is 20-50° C., and the reaction pressure is 0.05-0.3 MPa.

[0015] Preferably, the method further comprises passing the acetylene alcohol compounds obtained by the reaction into an aging hydrolysis kettle for aging hydrolysis, and then distilling the aging hydrolysis product to obtain refined acetylene alcohol compounds; and compressing the unreacted acetylene and returning it to the acetylene storage tank for recycling.

[0016] The beneficial effects of the present invention are: 1. The present invention connects the catalyst storage tank and the solvent storage tank with the emulsifier, so that the catalyst and the solvent can be emulsified into a slurry. The finer catalyst increases the contact area with the reaction materials, which can reduce the amount of catalyst used. By controlling the feed rate, the reaction can be carried out faster. In traditional kettle-type intermittent reactions, as the materials become thicker, the reaction becomes difficult to proceed, resulting in prolonged reaction time, significantly increased side reactions, and reduced production efficiency.

[0017] 2. The present invention arranges the discharge port of the reactor at the upper part of the reactor, the discharge port of the pipeline connecting the emulsifier and the reactor at the middle part of the reactor, and the mixer is connected with the bottom of the reactor, so that the mixture of acetylene and ketone is fed from the bottom of the reactor, and the slurry of catalyst and solvent is fed from the middle part of the reactor, thereby increasing the contact area of ​​the reaction materials and promoting the full reaction; at the same time, the reaction product overflows from the upper part of the reactor, so that a certain positive pressure is maintained in the reactor, further promoting the forward reaction, greatly shortening the reaction time, reducing the occurrence of side reactions, and making the reaction selectivity and conversion rate better than the traditional intermittent reactor production process.

[0018] 3. The present invention realizes continuous feeding reaction by connecting multiple reactors in series, thereby improving production efficiency and ensuring product yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.

[0020] Figure 1 It is a schematic diagram of a preparation device of an alkynol compound according to an embodiment of the present invention; In the figure, 1. catalyst storage tank; 11. first flow controller; 2. solvent storage tank; 21. second flow controller; 3. acetylene storage tank; 31. third flow controller; 4. ketone monomer storage tank; 41. fourth flow controller; 5. emulsifier; 6. mixer; 7. first reactor; 8. second reactor; 9. third reactor; 10. aging hydrolysis reactor. DETAILED DESCRIPTION

[0021] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0022] In the description of the embodiments of the present application, the term "plurality" refers to more than two (including two), and the orientation or positional relationship indicated by the technical terms "upper part", "middle part", "bottom part", etc. is based on the orientation or positional relationship shown in the accompanying drawings. In the description of the embodiments of the present application, unless otherwise clearly specified and limited, the technical terms "installation", "connection", "connection" and other terms should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral whole; it can also be a mechanical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the internal connection of two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the embodiments of the present application can be understood according to the specific circumstances.

[0023] First, please refer to Figure 1The embodiment of the present application provides a preparation device for alkynol compounds, including: a catalyst storage tank 1, a solvent storage tank 2, an acetylene storage tank 3, a ketone monomer storage tank 4, an emulsifier 5, a mixer 6, a first reactor 7, a second reactor 8, a third reactor 9 and an aging hydrolysis reactor 10. The catalyst storage tank 1 and the solvent storage tank 2 are connected to the emulsifier 5 through a pipeline, a first flow controller 11 is provided on the catalyst feed pipeline, and a second flow controller 21 is provided on the solvent feed pipeline, and the catalyst and the solvent are controlled to enter the emulsifier 5 at a certain speed by the first flow controller 11 and the second flow controller 21 respectively. The emulsifier 5 can be a high shear emulsifier or a colloid mill, which is used to uniformly disperse the catalyst in the solvent to form an emulsified slurry. The acetylene storage tank 3 and the ketone monomer storage tank 4 are connected to the mixer 6 through a pipeline; a third flow controller 31 is provided on the acetylene feed pipeline, and a fourth flow controller 41 is provided on the ketone monomer feed pipeline, and the third flow controller 31 and the fourth flow controller 41 are used to control the acetylene and the ketone monomer to enter the mixer 6 at a certain speed. The mixer 6 can be a static mixer for fully mixing the acetylene and the ketone monomer. The first flow controller 11, the second flow controller 21, the third flow controller 31 and the fourth flow controller 41 can adopt any device capable of controlling the material feed amount in the art, such as a metering pump, a star feed pump, an FIC, etc.

[0024] The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are arranged in series in sequence through pipelines, and the discharge port of the pipeline is located in the middle of each reactor. The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are all provided with stirring components, and they are all stainless steel reactors, which can greatly reduce the risk of acetylene explosion under high temperature and high pressure. The emulsifier 5 is connected to the first reactor 7 through a pipeline, and the discharge port of the pipeline is located in the middle of the first reactor 7, and the mixer 6 is connected to the bottom of the first reactor 7; the discharge ports of the first reactor 7, the second reactor 8 and the third reactor 9 are all located at the upper part of the reactor. Through the above arrangement, the catalyst slurry is fed from the middle of the first reactor 7, and the mixture of acetylene and ketone monomers is fed from the bottom of the first reactor 7, so as to increase the contact area of ​​the reaction materials and promote the reaction to proceed fully; at the same time, the acetylene compounds generated by the reaction and the unreacted acetylene overflow from the upper part of the first reactor 7 into the middle part of the second reactor 8, and the materials overflow from the upper part of the second reactor 8 to the middle part of the third reactor 9 to continue the reaction after the reaction, and at the same time, the reaction raw materials are continuously fed into the first reactor 7, so as to realize the continuous production of acetylene compounds and greatly improve the production efficiency. The reaction product overflowing from the upper part of the third reactor 9 enters the aging and hydrolysis kettle 10 for aging and hydrolysis to obtain the acetylene compound product.

[0025] In a second aspect, an embodiment of the present application provides a method for preparing an alkynol compound, which is implemented using the device described in the first aspect and specifically comprises the following steps: (1) Turn on the first flow controller 11 and the second flow controller 21 to control the catalyst and the solvent to enter the emulsifier 5 at a stable speed for homogenization and emulsification to obtain an emulsified slurry. The catalyst is a strong base, including but not limited to potassium hydroxide; the solvent is at least one of an ether compound, an alkane compound, and a benzene compound.

[0026] (2) The third flow controller 31 and the fourth flow controller 41 are turned on to respectively control the acetylene and ketone monomers to flow into the mixer 6 and mix them evenly to obtain a mixture.

[0027] (3) The mixed material is fed from the bottom of the first reactor 7, and the emulsified slurry is fed from the middle of the first reactor 7, so that acetylene and ketone monomers are stirred and reacted in the first reactor 7 at a temperature of 20-50°C and a pressure of 0.05-0.3 MPa, and the acetylene alcohol compounds generated by the reaction and unreacted acetylene overflow from the upper part of the first reactor 7. The molar ratio of the ketone monomer, acetylene and catalyst entering the first reactor 7 is 1: (0.5-1.5): (0.5-2), and the amount of the solvent used is 2-5 times the mass of the catalyst.

[0028] (4) The material overflowing from the upper part of the first reactor 7 enters the middle part of the second reactor 8 along the pipeline, and continues to react by stirring at a temperature of 20-50°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the second reactor 8.

[0029] (5) The material overflowing from the upper part of the second reactor 8 enters the middle part of the third reactor 9 along the pipeline, and continues to react by stirring at a temperature of 20-50°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the third reactor 9.

[0030] (6) The material overflowing from the upper part of the third reactor 9 enters the aging and hydrolysis reactor 10 along the pipeline, and the crude product is aged and hydrolyzed. The aged and hydrolyzed material is then continuously distilled to obtain acetylene alcohol compounds. The unreacted acetylene is compressed and returned to the acetylene storage tank for recycling.

[0031] The reaction principle of the present invention is as follows:

[0032] The device provided by the present invention can realize the continuous preparation of alkynol compounds, improve production efficiency, greatly reduce the amount of catalyst used, and is easy to control process parameters. The process reaction is stable and has high safety, and is suitable for industrial production.

[0033] In order to make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below.

[0034] Example 1 A method for preparing an alkynol compound, using Figure 1 The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are all 200 L stainless steel reactors, and specifically include the following steps: (1) Clean and dry the reaction device, then pass nitrogen gas through it to check for leaks and ensure that there are no leaks. Replace the air in the system so that the oxygen content online detector shows an oxygen concentration of <2%.

[0035] (2) Potassium hydroxide is added to the catalyst storage tank 1 and nitrogen is passed through it for protection. The first flow controller 11 is turned on to control the potassium hydroxide to be added to the emulsifier 5 at a rate of 50 kg / h.

[0036] (3) The second flow controller 21 is turned on to control the methyl tert-butyl ether to enter the emulsifier 5 at a rate of 100 kg / h. The potassium hydroxide and the solvent are homogenized and emulsified in the emulsifier 5 to obtain an emulsified slurry.

[0037] (4) Turn on the integrated cooling and heating machine and control the temperature of the jacket and built-in coil of the first reactor 7, the second reactor 8, and the third reactor 9 at 35°C.

[0038] (5) The emulsified slurry in the emulsifier 5 is fed into the first reactor 7 through a feed pipe inserted into the middle of the first reactor 7, and the stirring assembly in the first reactor 7 is turned on for stirring.

[0039] (6) The third flow controller 31 and the fourth flow controller 41 are turned on to control acetylene to enter the mixer 6 at a rate of 25 kg / h and methyl isobutyl ketone to enter the mixer 6 at a rate of 150 kg / h to be mixed evenly to obtain a mixture. The mixture is fed from the bottom of the first reactor 7, so that acetylene and methyl isobutyl ketone are stirred and reacted in the first reactor 7 at a temperature of 35°C and a pressure of 0.05-0.3 MPa. The acetylene alcohol compounds generated by the reaction and the unreacted acetylene overflow from the upper part of the first reactor 7. In the first reactor 7, the molar ratio of ketone, acetylene and potassium hydroxide is 1:0.63:0.54.

[0040] (7) The material overflowing from the upper part of the first reactor 7 enters the middle part of the second reactor 8 along the pipeline, and continues to react by stirring at a temperature of 35°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the second reactor 8.

[0041] (8) The material overflowing from the upper part of the second reactor 8 enters the middle part of the third reactor 9 along the pipeline, and continues to react by stirring at a temperature of 35° C. and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the third reactor 9.

[0042] (9) The material overflowing from the upper part of the third reaction kettle 9 enters the aging and hydrolysis kettle 10 along the pipeline, and the crude product is aged and hydrolyzed. Then, the aged and hydrolyzed material is continuously distilled to obtain an acetylene glycol product. After testing, the purity is 98.89% and the yield is 93.68%.

[0043] Example 2 A method for preparing an alkynol compound, using Figure 1 The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are all 200 L stainless steel reactors, and specifically include the following steps: (1) Clean and dry the reaction device, then pass nitrogen gas through it to check for leaks and ensure that there are no leaks. Replace the air in the system so that the oxygen content online detector shows an oxygen concentration of <2%.

[0044] (2) Potassium hydroxide is added to the catalyst storage tank 1 and nitrogen is passed through it for protection. The first flow controller 11 is turned on to control the potassium hydroxide to be added to the emulsifier 5 at a rate of 80 kg / h.

[0045] (3) The second flow controller 21 is turned on to control methyl tert-butyl ether to enter the emulsifier 5 at a rate of 200 kg / h. Potassium hydroxide and the solvent are homogenized and emulsified in the emulsifier 5 to obtain an emulsified slurry.

[0046] (4) Turn on the integrated cooling and heating machine and control the temperature of the jacket and built-in coil of the first reactor 7, the second reactor 8, and the third reactor 9 at 40°C.

[0047] (5) The emulsified slurry in the emulsifier 5 is fed into the first reactor 7 through a feed pipe inserted into the middle of the first reactor 7, and the stirring assembly in the first reactor 7 is turned on for stirring.

[0048] (6) The third flow controller 31 and the fourth flow controller 41 are turned on to control acetylene to enter the mixer 6 at a rate of 30 kg / h and methyl isobutyl ketone to enter the mixer 6 at a rate of 150 kg / h to obtain a mixed material. The mixed material is fed from the bottom of the first reactor 7, so that acetylene and methyl isobutyl ketone are stirred and reacted in the first reactor 7 at a temperature of 40°C and a pressure of 0.05-0.3 MPa. The acetylene alcohol compounds generated by the reaction and the unreacted acetylene overflow from the upper part of the first reactor 7. In the first reactor 7, the molar ratio of ketone, acetylene and potassium hydroxide is 1:0.76:0.86.

[0049] (7) The material overflowing from the upper part of the first reactor 7 enters the middle part of the second reactor 8 along the pipeline, and continues to react by stirring at a temperature of 40°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the second reactor 8.

[0050] (8) The material overflowing from the upper part of the second reactor 8 enters the middle part of the third reactor 9 along the pipeline, and continues to react by stirring at a temperature of 40° C. and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the third reactor 9.

[0051] (9) The material overflowing from the upper part of the third reaction kettle 9 enters the aging and hydrolysis kettle 10 along the pipeline, and the crude product is aged and hydrolyzed. Then, the aged and hydrolyzed material is continuously distilled to obtain an acetylene glycol product. After testing, the purity is 99.01% and the yield is 95.41%.

[0052] Example 3 A method for preparing an alkynol compound, using Figure 1 The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are all 200 L stainless steel reactors, and specifically include the following steps: (1) Clean and dry the reaction device, then pass nitrogen gas through it to check for leaks and ensure that there are no leaks. Replace the air in the system so that the oxygen content online detector shows an oxygen concentration of <2%.

[0053] (2) Potassium hydroxide is added to the catalyst storage tank 1 and nitrogen is passed through it for protection. The first flow controller 11 is turned on to control the potassium hydroxide to be added to the emulsifier 5 at a rate of 50 kg / h.

[0054] (3) The second flow controller 21 is turned on to control cyclohexane to enter the emulsifier 5 at a rate of 200 kg / h. Potassium hydroxide and the solvent are homogenized and emulsified in the emulsifier 5 to obtain an emulsified slurry.

[0055] (4) Turn on the integrated cooling and heating machine and control the temperature of the jacket and built-in coil of the first reactor 7, the second reactor 8, and the third reactor 9 at 50°C.

[0056] (5) The emulsified slurry in the emulsifier 5 is fed into the first reactor 7 through a feed pipe inserted into the middle of the first reactor 7, and the stirring assembly in the first reactor 7 is turned on for stirring.

[0057] (6) The third flow controller 31 and the fourth flow controller 41 are turned on to control acetylene to enter the mixer 6 at a rate of 20 kg / h and methyl isobutyl ketone to enter the mixer 6 at a rate of 150 kg / h to be mixed evenly to obtain a mixture. The mixture is fed from the bottom of the first reactor 7, so that acetylene and methyl isobutyl ketone are stirred and reacted in the first reactor 7 at a temperature of 50°C and a pressure of 0.05-0.3 MPa. The acetylene alcohol compounds generated by the reaction and the unreacted acetylene overflow from the upper part of the first reactor 7. In the first reactor 7, the molar ratio of ketone, acetylene and potassium hydroxide is 1:0.5:0.54.

[0058] (7) The material overflowing from the upper part of the first reactor 7 enters the middle part of the second reactor 8 along the pipeline, and continues to react by stirring at a temperature of 50° C. and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the second reactor 8.

[0059] (8) The material overflowing from the upper part of the second reactor 8 enters the middle part of the third reactor 9 along the pipeline, and continues to be stirred and reacted at a temperature of 50°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the third reactor 9.

[0060] (9) The material overflowing from the upper part of the third reaction kettle 9 enters the aging and hydrolysis kettle 10 along the pipeline, and the crude product is aged and hydrolyzed. Then, the aged and hydrolyzed material is continuously distilled to obtain an acetylene glycol product. The purity is 99.14% and the yield is 95.68%.

[0061] Example 4 A method for preparing an alkynol compound, using Figure 1 The first reactor 7, the second reactor 8, the third reactor 9 and the aging hydrolysis reactor 10 are all 200 L stainless steel reactors, and specifically include the following steps: (1) Clean and dry the reaction device, then pass nitrogen gas through it to check for leaks and ensure that there are no leaks. Replace the air in the system so that the oxygen content online detector shows an oxygen concentration of <2%.

[0062] (2) Potassium hydroxide is added to the catalyst storage tank 1 and nitrogen is passed through it for protection. The first flow controller 11 is turned on to control the potassium hydroxide to be added to the emulsifier 5 at a rate of 50 kg / h.

[0063] (3) The second flow controller 21 is turned on to control xylene to enter the emulsifier 5 at a rate of 240 kg / h. Potassium hydroxide and the solvent are homogenized and emulsified in the emulsifier 5 to obtain an emulsified slurry.

[0064] (4) Turn on the integrated cooling and heating machine and control the temperature of the jacket and built-in coil of the first reactor 7, the second reactor 8, and the third reactor 9 at 60°C.

[0065] (5) The emulsified slurry in the emulsifier 5 is fed into the first reactor 7 through a feed pipe inserted into the middle of the first reactor 7, and the stirring assembly in the first reactor 7 is turned on for stirring.

[0066] (6) The third flow controller 31 and the fourth flow controller 41 are turned on to control acetylene to enter the mixer 6 at a rate of 50 kg / h and methyl isobutyl ketone to enter the mixer 6 at a rate of 180 kg / h to obtain a mixed material. The mixed material is fed from the bottom of the first reactor 7, so that acetylene and methyl isobutyl ketone are stirred and reacted in the first reactor 7 at a temperature of 60°C and a pressure of 0.05-0.3 MPa. The acetylene alcohol compounds generated by the reaction and the unreacted acetylene overflow from the upper part of the first reactor 7. In the first reactor 7, the molar ratio of ketone, acetylene and potassium hydroxide is 1:1.05:0.45.

[0067] (7) The material overflowing from the upper part of the first reactor 7 enters the middle part of the second reactor 8 along the pipeline, and continues to react by stirring at a temperature of 60° C. and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the second reactor 8.

[0068] (8) The material overflowing from the upper part of the second reactor 8 enters the middle part of the third reactor 9 along the pipeline, and continues to react by stirring at a temperature of 60°C and a pressure of 0.05-0.3 MPa. The reacted material overflows from the upper part of the third reactor 9.

[0069] (9) The material overflowing from the upper part of the third reaction kettle 9 enters the aging and hydrolysis kettle 10 along the pipeline, and the crude product is aged and hydrolyzed. Then, the aged and hydrolyzed material is continuously distilled to obtain an acetylene glycol product. The purity is 99.26% and the yield is 95.13%.

[0070] It should be noted that the above embodiments all belong to the same inventive concept, and the description of each embodiment has its own focus. For matters that are not described in detail in some embodiments, reference may be made to the description in other embodiments.

[0071] The above-mentioned embodiments only express the implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A device for preparing acetylenic alcohol compounds, characterized in that: Including catalyst storage tanks, solvent storage tanks, acetylene storage tanks, ketone monomer storage tanks, emulsifiers, mixers and reactors; Wherein, the catalyst storage tank and the solvent storage tank are connected to the emulsifier, and the acetylene storage tank and the ketone monomer storage tank are connected to the mixer; the discharge port of the reactor is arranged at the upper part of the reactor, the emulsifier is connected to the reactor through a pipeline, and the discharge port of the pipeline is located in the middle part of the reactor, and the mixer is connected to the bottom of the reactor.

2. The preparation device of alkynol compounds according to claim 1, characterized in that: It also includes a first flow controller, a second flow controller, a third flow controller and a fourth flow controller; the first flow controller is arranged on the catalyst feed pipeline, the second flow controller is arranged on the solvent feed pipeline, the third flow controller is arranged on the acetylene feed pipeline, and the fourth flow controller is arranged on the ketone monomer feed pipeline.

3. The preparation device of alkynol compounds according to claim 1, characterized in that: There are multiple reactors, which are connected in series through pipelines, and the discharge ports of the pipelines are located in the middle of the reactors.

4. The preparation device of alkynol compounds according to claim 1, characterized in that: A stirring assembly is arranged in the reactor; the reactor is a stainless steel reactor.

5. The preparation device of alkynol compounds according to claim 1, characterized in that: It also includes an aging hydrolysis kettle, which is connected to the discharge port of the reaction kettle.

6. A method for preparing an alkynol compound, characterized in that: Using the preparation device of the alkynol compound according to any one of claims 1 to 5, the preparation method comprises the following steps: Passing the catalyst and the solvent into an emulsifier for homogenization and emulsification to obtain an emulsified slurry; The acetylene and ketone monomers are introduced into a mixer and mixed evenly to obtain a mixture; The mixed material is fed from the bottom of the reactor, and the emulsified slurry is fed from the middle of the reactor, so that acetylene and ketone monomers are fully reacted in the reactor, and the acetylene alcohol compounds generated by the reaction and unreacted acetylene overflow from the upper part of the reactor.

7. The method for preparing an alkynol compound according to claim 6, characterized in that: The molar ratio of the ketone monomer, acetylene and catalyst is 1: (0.5-1.5): (0.5-2), and the amount of the solvent used is 2-5 times the mass of the catalyst.

8. The method for preparing an alkynol compound according to claim 6, characterized in that: The catalyst is a strong base, and the solvent is at least one of an ether compound, an alkane compound, and a benzene compound.

9. The method for preparing an alkynol compound according to claim 6, wherein The reaction temperature is 20-50° C., and the reaction pressure is 0.05-0.3 MPa.

10. The method for preparing an alkynol compound according to claim 6, characterized in that: The method also includes passing the acetylene alcohol compounds obtained by the reaction into an aging hydrolysis kettle for aging hydrolysis, and then distilling the aging hydrolysis products to obtain refined acetylene alcohol compounds; and compressing the unreacted acetylene and returning it to the acetylene storage tank for recycling.

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