阅读说明：本技术 呋喃酮提纯用冷却结晶设备 (Cooling crystallization equipment for purifying furanone ) 是由 王玉斌 李炳亮 赵程成 姜维强 孙多龙 刘兴然 于 2019-10-25 设计创作，主要内容包括：本发明涉及一种呋喃酮提纯用的冷却结晶设备,包括预冷结晶罐和结晶反应器,使用流程为将含有呋喃酮半成品的高温浓缩溶液泵入预冷结晶罐中预冷结晶,然后进入结晶反应器中冷却结晶。通过预冷降低了冷媒的使用量,从而降低能源的消耗,同时使用振动技术和冷却结晶后的分离技术,减少了后续处理的步骤,提高了结晶的质量和结晶的效率,使得结晶的效果和过程可控,具有较大的使用价值。(The invention relates to a cooling crystallization device for purifying furanone, which comprises a precooling crystallization tank and a crystallization reactor, wherein the using process comprises the steps of pumping a high-temperature concentrated solution containing a furanone semi-finished product into the precooling crystallization tank for precooling crystallization, and then feeding the solution into the crystallization reactor for cooling crystallization. The use amount of the refrigerant is reduced through precooling, so that the energy consumption is reduced, and meanwhile, the vibration technology and the separation technology after cooling crystallization are used, so that the steps of subsequent treatment are reduced, the crystallization quality and the crystallization efficiency are improved, the crystallization effect and the crystallization process are controllable, and the use value is high.)

1. The utility model provides a furanone purification is with cooling crystallization equipment, includes precooling crystallizer (1) and crystallization reactor (2), its characterized in that: pumping the high-temperature concentrated solution containing the furanone semi-finished product into a precooling crystallization tank (1) for precooling crystallization, and then, cooling and crystallizing in a crystallization reactor; the precooling crystallization tank adopts a jacketed reaction tank, circulating cooling water is introduced into an interlayer for cooling crystallization, so that the temperature of the furanone mother liquor is reduced to 35-40 ℃, precooling mother liquor and part of furanone crystals are obtained, then the precooled mother liquor containing the crystals is subjected to centrifugal separation, the furanone crystals and a first solution are obtained, and the first solution is pumped into a cooling crystallization reactor (2) through a high-pressure pump; the crystallization reactor is of a cylindrical tower structure, the top of the crystallization reactor is provided with a semi-ellipsoidal top cover (3) for sealing, the top cover is provided with an opening (4), a precooled solution enters the crystallization reactor through a conveying pipe (5), one end of the conveying pipe, which is connected with the crystallization reactor, is of an L-shaped shape, the short edge of the L-shaped shape is inserted into the top of the crystallization reactor for a certain depth through the opening of the top cover, an impeller (6) is arranged inside the outlet of the conveying pipe, and blades of the impeller rotate under the impact of high-pressure liquid flow to generate a certain stirring effect; the reactor is a continuous crystallizer, three crystallizers (7) with the same structure are vertically arranged in the reactor, the structures of the crystallizers adopt an interlayer arrangement, a refrigerant pipe is spirally arranged on an inner cylinder of the reactor, a refrigerant discharged from a compressor enters from the bottom of the crystallizer at the bottommost part, flows out from the top of the crystallizer at the top part, and then returns to the compressor; the crystallizer comprises a crystallizing cylinder (8) and a separating cylinder (9), the separating cylinder is arranged at the lower part of the crystallizing cylinder, the bottom of the crystallizing cylinder is of a conical structure, an electric control valve (10) is arranged at the bottommost end, a centrifugal separation mechanism is arranged in the separating cylinder, a second solution and a furanone crystal which are further cooled are obtained after separation, the furanone crystal is taken out from a discharge port, and the second solution enters the crystallizer arranged at the lower layer for further cooling and crystallization.

2. The cooling crystallization device for furanone purification according to claim 1, wherein: the inner wall of the crystallizer is fixedly provided with a vibrator, the vibration frequency of the vibrator can be adjusted, and the vibrator can be an ultrasonic vibrator.

3. The cooling crystallization device for furanone purification according to claim 1, wherein: and a temperature detection device is arranged in the crystallizer so as to detect the specific condition of the crystallization reaction in real time.

Technical Field

The invention relates to cooling crystallization equipment for purifying furanone, and belongs to the technical field of chemical equipment.

Background

The furanone natural product exists in strawberry, oat, cheese, cooked beef, beer, cocoa, coffee, tea, mango, lychee, malt, gooseberry, grape, heated beef, pineapple and the like, and in 1965, the furanone is firstly separated from the ether extract of pineapple juice, and the molecular structural formula of the furanone is determined. Furanone has intense caramel taste, low fragrance threshold value and obvious fragrance effect, and is widely used as an additive for food, tobacco, beverage and the like. The process for preparing furanone by using methylglyoxal mainly comprises the following steps: and (3) preparing intermediate hexanedione through coupling reaction of methylglyoxal, acetic acid and zinc powder, extracting and purifying, then performing cyclization reaction with disodium hydrogen phosphate to obtain furanone, and separating and purifying to obtain a furanone finished product. However, the purification of furanones is a critical step that limits the quality of the final product.

In chemical production, crystallization is a common chemical operation unit, and the main modes of crystallization include: 1. cooling, cooling and crystallizing, wherein a refrigerant enters a crystallization kettle jacket to exchange heat with materials in the kettle, and the purpose of cooling and crystallizing is achieved; 2. cooling and crystallizing by a heat exchanger, wherein a refrigerant passes through a shell pass of the heat exchanger, and a material circulates in a tube pass by a circulating pump, so that cooling and crystallizing are performed; 3. evaporating and crystallizing, namely evaporating the material through steam to reach the process that the concentration of the material is increased and crystals are separated out; 4. vacuum flash evaporation crystallization is carried out, wherein a high-pressure steam jet pump is used for carrying out the process that the crystallization tank is in negative pressure, the flash evaporation moisture of the material is reduced when the temperature is reduced, and the material is crystallized. In the cooling crystallization process, the material concentration, the material temperature, the heat transfer temperature difference, the heat transfer rate, the stirring form and the stirring speed have great influence on the quality of the crystallized material, and the crystallization process is difficult to control. When the jacket crystallizing tank is adopted, the inner wall of the crystallizing tank is easy to scale, the heat transfer and the product quality are influenced, meanwhile, the supersaturation degree of the tank wall is large, the secondary nucleation amount in the process is large, and the obtained crystal particles are fine and the crystal form is poor.

Disclosure of Invention

The invention aims to provide cooling crystallization equipment suitable for furanone purification, which is reasonably designed by adopting advanced technology in modern industrial technology and combining the cooling crystallization principle so as to improve the efficiency and quality of the furanone purification process.

The invention is realized by the following technical scheme:

the utility model provides a furanone purification is with cooling crystallization equipment, includes precooling crystallizer 1 and crystallization reactor 2, its characterized in that: pumping the concentrated high-temperature furanone solution into a precooling crystallization tank, wherein the precooling crystallization tank adopts a jacketed reaction tank, circulating cooling water is introduced into an interlayer for cooling crystallization, so that the temperature of the furanone mother solution is reduced to 35-40 ℃, precooling mother solution and part of furanone crystals are obtained, then carrying out centrifugal separation to obtain furanone crystals and a first solution, and then pumping the furanone crystals and the first solution into a cooling crystallization reactor through a high-pressure pump. The crystallization reactor is of a cylindrical tower structure, the top of the crystallization reactor is provided with a semi-ellipsoidal top cover 3 seal, the top cover is provided with an opening 4, a pre-cooled solution I enters the crystallization reactor through a conveying pipe 5, one end of the conveying pipe, which is connected with the crystallization reactor, is in an L-shaped arrangement, the short edge of the L-shaped arrangement is inserted into the top of the crystallization reactor through the opening of the top cover for a certain depth, an impeller is arranged inside the outlet of the conveying pipe, and the blades of the impeller rotate under the impact of high-pressure liquid flow to generate a certain stirring effect. The reactor is a continuous crystallizer, three crystallizers with the same structure are vertically arranged inside the reactor, the structure of each crystallizer is arranged by an interlayer, a refrigerant pipe is spirally arranged on an inner cylinder of the reactor, a refrigerant coming out of the compressor enters from the bottom of the reactor and flows out from the top of the reactor and returns to the compressor, each crystallizer comprises a crystallizing cylinder and a separating cylinder, the separating cylinder is arranged at the lower part of the crystallizing cylinder, the bottom of the crystallizing cylinder is of a conical structure, an electric control valve is arranged at the lowest end of the crystallizing cylinder, a centrifugal separation mechanism is arranged inside the separating cylinder, a second solution and a furanone crystal which are further cooled are obtained after separation, the furanone crystal is taken out from a discharge port, and the second solution enters the crystallizer arranged at the lower layer for further cooling and crystallization.

Furthermore, in order to prevent the solution from generating crystal scale on the inner wall of the crystallizer, a vibrator is fixedly arranged on the inner wall of the crystallizer, the vibration frequency of the vibrator can be adjusted, and the vibrator is an ultrasonic vibrator.

Further, a temperature detection device is arranged inside the crystallizer so as to detect the specific condition of the crystallization reaction.

The invention has the following beneficial effects;

1. the water with lower use cost is used for precooling, so that the use amount of the refrigerant is reduced, the cost is reduced, and the energy consumption is saved.

2. The vibrator is arranged in the crystallizer, a stirring device and a wall scraping device in the traditional process equipment are omitted, the complexity of the equipment is reduced, the manufacturing cost is reduced, the control is simpler and more convenient, and the uniform cooling crystallization can be realized through the control of the vibration frequency.

3. The crystallization and separation structure are integrated, so that the liquid containing crystals and coming out of the crystallization cylinder is not required to be separated by separately arranging additional processes, the treatment processes are reduced, and the crystallization efficiency is improved.

4. Through the setting of tertiary crystallizer, continuous cooling crystallization compares and lasts the crystallization under a temperature, and efficiency is higher, and the crystallization effect is better.

Drawings

FIG. 1 is a schematic structural diagram of a furanone cooling crystallizer of the present invention.

In the figure: 1-precooling a crystallizing tank; 2-a crystallization reactor; 3-a top cover; 4-opening; 5-conveying pipe; 6-impeller; 7-a crystallizer; 8-a crystallization cylinder; 9-a separation cylinder; 10-electrically controlled valve.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

A cooling crystallization device for furanone purification comprises a precooling crystallization tank 1 and a crystallization reactor 2, wherein a high-temperature concentrated solution containing a furanone semi-finished product is pumped into the precooling crystallization tank 1, a jacketed reaction tank is adopted in the precooling crystallization tank, the jacketed reaction tank is a device commonly used in the field, the specific structure is not described in detail, circulating cooling water is introduced into an interlayer for cooling crystallization, so that the temperature of a furanone mother solution is reduced to 35-40 ℃, and the precooling mother solution and a part of furanone crystals are obtained. The circulating water with low cost is utilized for primary cooling, so that the temperature of the furanone mother liquor is reduced to 35-40 ℃, the usage amount of a refrigerant is reduced for subsequent cooling crystallization, and the cost and the energy consumption are reduced. And (3) carrying out centrifugal separation on the mother liquor containing the crystals after precooling to obtain furanone crystals and a first solution, and pumping the precooled first solution into a cooling crystallization reactor 2 through a high-pressure pump.

The crystallization reactor is of a cylindrical tower structure, the top of the crystallization reactor is provided with a semi-ellipsoidal top cover 3 for sealing, the top cover is provided with an opening 4, a pre-cooled solution I enters the crystallization reactor through a conveying pipe 5, one end of the conveying pipe, which is connected with the crystallization reactor, is of an L-shaped shape, the short edge of the L-shaped shape is inserted into the top of the crystallization reactor through the opening of the top cover for a certain depth, an impeller 6 is arranged inside the outlet of the conveying pipe, and blades of the impeller rotate under the impact of high-pressure liquid flow to generate a certain stirring effect. The reactor is a continuous crystallizer, three crystallizers 7 with the same structure are vertically arranged inside the reactor, the structures of the crystallizers adopt interlayer arrangement, refrigerant pipes are spirally arranged on the inner cylinder of the reactor, refrigerants coming out of the compressor enter from the bottom of the crystallizer at the bottommost part and flow out from the top of the crystallizer at the top, and then return to the compressor, so that the arrangement can ensure that the temperature of the solution is gradually reduced from the crystallizer at the top, and the temperature of the crystallizer at the bottommost part is lowest.

The structure of crystallizer contains a crystallization section of thick bamboo 8 and a knockout drum 9, and the knockout drum setting is in the lower part of a crystallization section of thick bamboo, and the bottom of a crystallization section of thick bamboo is coniform structure to set up an automatically controlled valve 10 at the lower extreme, the inside centrifugal separation mechanism that is provided with of knockout drum obtains solution two and the furanone crystal of further cooling after the separation, and the furanone crystal is taken out from the discharge gate, and solution two gets into the crystallizer of lower floor setting in further cooling crystallization.

Further, in order to prevent the solution from generating crystal scale on the inner wall of the crystallizer, a vibrator is fixedly arranged on the inner wall of the crystallizer, the vibration frequency of the vibrator can be adjusted, and the vibrator can be selected from an ultrasonic vibrator.

Further, a temperature detection device is arranged inside the crystallizer so as to detect the specific condition of the crystallization reaction.

In the description of the present specification, reference to the description of the term "specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.