CN114671773A - A kind of high-yield cyclic acid synthesis method - Google Patents

A kind of high-yield cyclic acid synthesis method Download PDF

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CN114671773A
CN114671773A CN202210488611.XA CN202210488611A CN114671773A CN 114671773 A CN114671773 A CN 114671773A CN 202210488611 A CN202210488611 A CN 202210488611A CN 114671773 A CN114671773 A CN 114671773A
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刘为祥
李兴君
章志成
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Jiangxi Zhaoyang Technology Co ltd
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/16Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions not involving the amino or carboxyl groups
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
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    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
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Abstract

本发明属于环酸合成技术领域,尤其是一种高收率环酸合成方法,针对目前的反应釜缺乏专门的催化氢化结构,氢气加入后反应的时间长,氢化效果不佳,现提出以下方案,将质量分数5‑7%的硫酸溶液、铂类催化剂和预处理后的氨甲苯酸按照重量比2:1:6的量从合成机构的进料口加入反应釜本体中,关闭反应釜本体的进料口,启动装置;加热板通电后电热棒对反应釜本体内的溶液进行加热,待反应液温度达到预设温度后,电动机带动轴杆转动,搅拌组件对反应液进行混合搅拌。

Figure 202210488611

The invention belongs to the technical field of cyclic acid synthesis, in particular to a high-yield cyclic acid synthesis method. In view of the fact that the current reaction kettle lacks a special catalytic hydrogenation structure, the reaction time after hydrogen is added is long, and the hydrogenation effect is not good, the following scheme is now proposed. , add the sulfuric acid solution of 5-7% mass fraction, platinum-based catalyst and pretreated aminotoluic acid from the feed port of the synthesis mechanism into the reactor body according to the weight ratio of 2:1:6, and close the reactor body After the heating plate is energized, the electric heating rod heats the solution in the reactor body. When the temperature of the reaction liquid reaches the preset temperature, the motor drives the shaft to rotate, and the stirring component mixes and stirs the reaction liquid.

Figure 202210488611

Description

一种高收率环酸合成方法A kind of high-yield cyclic acid synthesis method

技术领域technical field

本发明涉及环酸合成技术领域,尤其涉及一种高收率环酸合成方法。The invention relates to the technical field of cyclic acid synthesis, in particular to a high-yield cyclic acid synthesis method.

背景技术Background technique

氨甲环酸,又名传明酸、凝血酸、止血环酸,分子式为C8H15NO2,化学名为反-4-氨甲基环已烷甲酸,为白色结晶性粉末,无臭,味微,在水中易溶,在乙醇、丙酮、三氯甲烷或乙醚中几乎不溶。Tranexamic acid, also known as tranexamic acid, tranexamic acid, hemostatic acid, molecular formula is C8H15NO2, chemical name is trans-4-aminomethylcyclohexanecarboxylic acid, it is a white crystalline powder, odorless, slight taste, in Soluble in water, almost insoluble in ethanol, acetone, chloroform or ether.

氨甲环酸在医疗制药方面具有及其广泛的作用,可以安全可靠地降低创伤出血患者的死亡率;能够降低颅脑患者发生进行性出血的可能;能够显著降低经血过多妇女的血量损失;能够使产后出血量显著地减少;能够降低术后输血的风险并减少了术中和术后的出血量,能够用于因子Ⅷ缺乏的血友病患者手术前后的辅助治疗同时还具有退黑除斑的功效。Tranexamic acid has a wide range of effects in medicine and pharmacy. It can safely and reliably reduce the mortality rate of traumatic hemorrhage patients; it can reduce the possibility of progressive bleeding in patients with craniocerebral brain; it can significantly reduce blood loss in women with excessive menstrual bleeding It can significantly reduce the amount of postpartum hemorrhage; it can reduce the risk of postoperative blood transfusion and reduce the amount of intraoperative and postoperative bleeding, and can be used for the adjuvant treatment of factor VIII deficiency hemophilia patients before and after surgery. Spot removal effect.

氨甲环酸在生产加工过程中需要对半成品进行催化氢化以得到所需的加氢产物,通常此过程是在反应釜中进行,但是由于目前的反应釜缺乏专门的催化氢化结构,氢气加入后反应的时间长,氢化效果不佳。Tranexamic acid needs to carry out catalytic hydrogenation on the semi-finished product in the production and processing process to obtain the desired hydrogenated product. Usually this process is carried out in a reaction kettle. However, due to the lack of a special catalytic hydrogenation structure in the current reaction kettle, after hydrogen is added The reaction time is long and the hydrogenation effect is not good.

发明内容SUMMARY OF THE INVENTION

本发明提出的一种高收率环酸合成方法,包括以下步骤:A kind of high-yield cyclic acid synthesis method proposed by the present invention comprises the following steps:

一种高收率环酸合成方法,包括以下步骤:A high-yield cyclic acid synthesis method, comprising the following steps:

步骤一:将氨甲苯酸与纯水按照重量比1:5混合,在搅拌条件下缓慢加入浓硫酸,加热至预设温度,氨甲苯酸溶解,冷却结晶,过滤得到预处理后的氨甲苯酸,随后将质量分数5-7%的硫酸溶液、铂类催化剂和预处理后的氨甲苯酸按照重量比2:1:6的量从合成机构的进料口加入反应釜本体中,关闭反应釜本体的进料口,启动装置;Step 1: Mix aminotoluic acid and pure water in a weight ratio of 1:5, slowly add concentrated sulfuric acid under stirring conditions, heat to a preset temperature, dissolve aminotoluic acid, crystallize by cooling, and filter to obtain pretreated aminotoluic acid , then add 5-7% mass fraction of sulfuric acid solution, platinum-based catalyst and pretreated aminotoluic acid from the feed port of the synthesis mechanism into the reactor body according to the weight ratio of 2:1:6, and close the reactor. The feed port of the body, the starting device;

步骤二:加热板通电后电热棒对反应釜本体内的溶液进行加热,待反应液温度达到预设温度后,电动机带动轴杆转动,搅拌组件对反应液进行混合搅拌;Step 2: After the heating plate is energized, the electric heating rod heats the solution in the reactor body, and after the temperature of the reaction solution reaches the preset temperature, the motor drives the shaft to rotate, and the stirring component mixes and stirs the reaction solution;

具体搅拌过程中,随着六角轴座的转动,搅拌杆受到内部反应液的反向作用力和轴杆转动的驱动力,弹簧底座(会发生晃动带动搅拌杆振动,振动过程中搅拌杆能够增加与反应液的接触效果,提高搅拌组件的整体搅拌混合效果;During the specific stirring process, with the rotation of the hexagonal shaft seat, the stirring rod is subjected to the reverse force of the internal reaction liquid and the driving force of the rotation of the shaft rod. The contact effect with the reaction liquid improves the overall stirring and mixing effect of the stirring component;

步骤三:从进气管输送氢气至反应釜本体的内部,输送定量氢气后关闭进气管的阀门,制成加氢产物,然后再加入加氢产物重量比:的氢氧化钙,继续反应处理;Step 3: transport hydrogen from the gas inlet pipe to the inside of the reactor body, close the valve of the gas inlet pipe after transporting a certain amount of hydrogen to make a hydrogenated product, then add the calcium hydroxide of the hydrogenated product weight ratio: : , and continue the reaction treatment;

氢气输送过程,氢气进入回气座并从气孔中喷出,直接作用在反应溶液中,氢气在反应液中形成气泡,增加了气体与反应液之间的接触效果,提高催化氢化效果,微型气泵工作利用吸气管和进气槽对反应釜本体的内部进行吸气操作,并通过输气管进入回气座内,从气孔喷出,循环如此提高氢气与反应液的接触效果,反应结束后打开排气管阀门排出反应釜内部的气体,随后将反应后的溶液排出进行后续的转位反应;In the process of hydrogen delivery, hydrogen enters the return gas seat and is ejected from the air hole, and acts directly on the reaction solution. The hydrogen forms bubbles in the reaction solution, which increases the contact effect between the gas and the reaction solution, and improves the effect of catalytic hydrogenation. Micro air pump The work uses the suction pipe and the gas inlet groove to inhale the inside of the reactor body, and enters the return gas seat through the gas pipe, and sprays out from the air hole. The circulation improves the contact effect of the hydrogen and the reaction liquid. The exhaust pipe valve discharges the gas inside the reactor, and then discharges the reacted solution for subsequent transposition reaction;

步骤四:催化氢化反应期间,反应釜内部通入氢气,内部的压强会增大,催化氢化反应的效果会降低,而调压组件能够改变反应釜本体内部的压强,当氢气通入后,气流控制阀会进行排气操作,将气囊中的气体向外排出,气囊于气筒中收缩体积,推压底板向上移动,复位弹簧受到弹性形变后的反向作用力来辅助推压底板复位,进而完成高收率的环酸合成;Step 4: During the catalytic hydrogenation reaction, hydrogen is introduced into the reactor, the internal pressure will increase, and the effect of the catalytic hydrogenation reaction will be reduced, and the pressure regulating component can change the pressure inside the reactor body. The control valve will perform an exhaust operation to discharge the gas in the air bag to the outside, the air bag will shrink in volume in the air cylinder, push the bottom plate to move upward, and the return spring will receive the reverse force after elastic deformation to assist the push bottom plate to reset, and then complete High yield cyclic acid synthesis;

合成机构包括反应釜本体,所述反应釜本体的内部设置有回气组件,且回气组件包括回气座和气环,所述回气座的一侧外壁与反应釜本体的内壁之间固定连接,且回气座上设置有排气板,排气板上呈圆周等距开设有多个气孔,所述气环位于回气座的上方,气环与反应釜本体的内壁之间固定连接,且气环上开设有多个呈圆周等距的圆孔,圆孔的内壁固定连接有吸气管,吸气管的另一端均固定连接有进气槽,所述气环与回气座之间固定连接有两个输气管,且两个输气管上均设置有微型气泵。The synthesis mechanism includes a reaction kettle body, the interior of the reaction kettle body is provided with a gas return component, and the gas return component includes a gas return seat and a gas ring, and an outer wall of one side of the gas return seat is fixedly connected with the inner wall of the reactor body. , and the air return seat is provided with an exhaust plate, and the exhaust plate is provided with a plurality of air holes at equal distances around the circumference. The air ring is located above the air return seat, and the air ring is fixedly connected with the inner wall of the reactor body. And the air ring is provided with a plurality of circular holes that are equidistant around the circumference, the inner wall of the circular holes is fixedly connected with a suction pipe, and the other end of the suction pipe is fixedly connected with an air inlet groove, and the air ring and the return air seat are fixed. Two gas delivery pipes are fixedly connected between the two gas delivery pipes, and a micro air pump is arranged on the two gas delivery pipes.

优选地,所述回气座上固定连接有进气管,进气管的另一端穿过反应釜本体与外界的气管固定连接,且反应釜本体上开设有圆孔,圆孔位于气环的上方,圆孔的内壁固定连接有排气管。Preferably, an air inlet pipe is fixedly connected to the air return seat, the other end of the air inlet pipe is fixedly connected to the outside air pipe through the reactor body, and the reactor body is provided with a circular hole, and the circular hole is located above the gas ring, An exhaust pipe is fixedly connected to the inner wall of the round hole.

优选地,所述反应釜本体的外壁固定连接有三个呈圆周等距的支座,支座上均固定连接有支撑腿,且反应釜本体的上方设置有顶盖,反应釜本体的下方设置有底盒,底盒上开设有漏孔,漏孔的内壁固定连接有排料管。Preferably, the outer wall of the reactor body is fixedly connected with three supports that are equidistant around the circumference, and support legs are fixedly connected to the supports, and the top of the reactor body is provided with a top cover, and the bottom of the reactor body is provided with The bottom box is provided with a leak hole, and the inner wall of the leak hole is fixedly connected with a discharge pipe.

优选地,所述反应釜本体的内部设置有控温组件,控温组件位于回气座的下方,控温组件包括加热板和螺旋调温管,加热板与反应釜本体的内壁之间固定连接,加热板上设置有多个圆周等距的电热棒,且反应釜本体上开设有两个圆孔,两个圆孔的内壁分别固定连接有进水管和出水管,进水管和出水管分别与螺旋调温管的两端固定连接。Preferably, the inside of the reaction kettle body is provided with a temperature control assembly, the temperature control assembly is located below the air return seat, the temperature control assembly includes a heating plate and a spiral temperature regulating pipe, and the heating plate is fixedly connected to the inner wall of the reaction kettle body. , a plurality of electric heating rods with equidistant circumferences are arranged on the heating plate, and two circular holes are opened on the reactor body. The inner walls of the two circular holes are respectively fixed with a water inlet pipe and a water outlet pipe. Both ends of the spiral thermostat are fixedly connected.

优选地,所述顶盖的上侧外壁固定连接有机架,机架的内壁固定连接有电动机,电动机的输出端通过联轴器连接有轴杆,且轴杆的另一端穿过顶盖,轴杆的外部设置有搅拌组件,顶盖上开设有进料口。Preferably, a frame is fixedly connected to the upper outer wall of the top cover, a motor is fixedly connected to the inner wall of the frame, an output end of the motor is connected to a shaft through a coupling, and the other end of the shaft passes through the top cover, The outside of the shaft is provided with a stirring component, and the top cover is provided with a feeding port.

优选地,所述搅拌组件包括六角轴座和多个支杆,六角轴座上开设有六角凹槽,六角凹槽的内壁与轴杆的外壁之间固定连接,且多个支杆与六角轴座之间固定连接,多个支杆呈圆周等距分布。Preferably, the stirring assembly includes a hexagonal shaft seat and a plurality of support rods, the hexagonal shaft seat is provided with a hexagonal groove, the inner wall of the hexagonal groove and the outer wall of the shaft rod are fixedly connected, and the plurality of support rods are connected to the hexagonal shaft. The seats are fixedly connected, and a plurality of struts are distributed at equal distances around the circumference.

优选地,多个所述支杆上均开设有三个等距的圆孔,三个圆孔的内壁均固定连接有弹簧底座,且弹簧底座的顶端均固定连接有搅拌杆。Preferably, three equidistant circular holes are formed on each of the plurality of supporting rods, the inner walls of the three circular holes are fixedly connected with spring bases, and the top ends of the spring bases are fixedly connected with stirring rods.

优选地,所述顶盖上开设有两个对称的溢气孔,且两个溢气孔的内部均设置有调压组件。Preferably, the top cover is provided with two symmetrical air relief holes, and the inside of the two air relief holes are provided with pressure regulating components.

优选地,所述调压组件包括气筒和气囊,气筒的外壁与溢气孔的内壁之间固定连接,且气囊位于气筒的内部,气筒的顶部固定连接有气流控制阀,气流控制阀与气囊之间通过短管连接。Preferably, the pressure regulating assembly includes an air cylinder and an air bag, the outer wall of the air cylinder and the inner wall of the air outlet are fixedly connected, and the air bag is located inside the air cylinder, and the top of the air cylinder is fixedly connected with an air flow control valve, between the air control valve and the air bag Connect by short tube.

优选地,所述气囊的内部设置有推压底板,且气囊的顶部内壁固定连接有内附座,内附座的下侧外壁固定连接有复位弹簧,复位弹簧的另一端与推压底板之间固定连接。Preferably, the inside of the airbag is provided with a pushing bottom plate, the inner wall of the top of the airbag is fixedly connected with an inner attachment seat, the lower side outer wall of the inner attachment seat is fixedly connected with a return spring, and the other end of the return spring is between the pushing bottom plate and the inner attachment seat. Fixed connection.

本发明中的有益效果为:The beneficial effects in the present invention are:

1、本发明通过设置的反应釜本体、回气座、气环、排气板、气孔、吸气、进气槽、输气管和微型气泵,装置利用回气组件能够直接将输入的氢气进行输送至反应液中,从而产生气泡增加氢气与反应液之间的接触效果,同时在反应过程中,利用微型气泵对反应釜本体中的气体重复输送至反应液中,进一步提高氢气输送至反应釜本体后与内部反应液之间的反应效果;氢气输送过程,氢气进入回气座并从气孔中喷出,直接作用在反应溶液中,氢气在反应液中形成气泡,进一步增加了气体与反应液之间的接触效果,从而提高催化氢化效果。1. In the present invention, the reactor body, the gas return seat, the gas ring, the exhaust plate, the air hole, the suction, the air inlet groove, the gas transmission pipe and the micro air pump are provided, and the device can directly transport the input hydrogen by using the gas return component. into the reaction liquid, thereby generating bubbles to increase the contact effect between the hydrogen and the reaction liquid. At the same time, during the reaction process, the gas in the reaction kettle body is repeatedly transported to the reaction liquid by using a micro air pump, which further improves the delivery of hydrogen to the reaction kettle body. The reaction effect between the latter and the internal reaction solution; during the hydrogen delivery process, the hydrogen enters the return gas seat and is ejected from the air hole, and acts directly on the reaction solution, and the hydrogen forms bubbles in the reaction solution, which further increases the relationship between the gas and the reaction solution. The contact effect between the two, thereby improving the catalytic hydrogenation effect.

2、本发明通过设置的控温组件,加热板通电后电热棒对反应釜本体内的溶液进行加热,使得待反应液温度达到预设温度,满足反应所需的条件,螺旋调温管内通入调温液体(水),随着反应时间的加长或者加热板加热过度,反应液的温度超过预设值,将水从进水管输入,出水管送出,对反应液进行降温操作,避免温度过高影响反应的整体进程。2. In the present invention, the solution in the reactor body is heated by the electric heating rod after the heating plate is energized, so that the temperature of the liquid to be reacted reaches the preset temperature and meets the conditions required for the reaction. Warm liquid (water), with the prolongation of the reaction time or the excessive heating of the heating plate, the temperature of the reaction liquid exceeds the preset value, the water is input from the water inlet pipe, and the water outlet pipe is sent out, and the reaction liquid is cooled to avoid the influence of excessive temperature. the overall process of the reaction.

3、本发明通过设置搅拌组件,电动机带动轴杆转动,搅拌组件对反应液进行混合搅拌;搅拌过程中,随着六角轴座的转动,搅拌杆受到内部反应液的反向作用力和轴杆转动的驱动力,弹簧底座会发生晃动带动搅拌杆振动,振动过程中搅拌杆能够增加与反应液的接触效果,从而提高搅拌组件的整体搅拌混合效果。3. In the present invention, a stirring assembly is provided, the motor drives the shaft to rotate, and the stirring assembly mixes and stirs the reaction liquid; during the stirring process, with the rotation of the hexagonal shaft seat, the stirring rod is subjected to the reverse force of the internal reaction liquid and the shaft rod. With the driving force of rotation, the spring base will shake and drive the stirring rod to vibrate. During the vibration process, the stirring rod can increase the contact effect with the reaction liquid, thereby improving the overall stirring and mixing effect of the stirring assembly.

4、本发明通过设置的调压组件,催化氢化反应期间,由于反应釜内部通入氢气,其内部的压强会增大,从而催化氢化反应的效果会降低(气压增大后氢气的溶解度降低),而调压组件能够改变反应釜本体内部的压强,当氢气通入后,气流控制阀会进行排气操作,将气囊中的气体向外排出(初始时气囊中充入外界的空气使其膨胀),气囊于气筒中收缩体积,推压底板向上移动,复位弹簧受到弹性形变后的反向作用力来辅助推压底板复位。4. During the catalytic hydrogenation reaction, the pressure inside the reactor will increase due to the introduction of hydrogen into the reactor, so that the effect of the catalytic hydrogenation reaction will decrease (the solubility of hydrogen decreases after the pressure increases). , and the pressure regulating component can change the pressure inside the reactor body. When the hydrogen is introduced, the air flow control valve will perform an exhaust operation to discharge the gas in the air bag to the outside (the air bag is initially filled with outside air to expand it. ), the air bag shrinks in the air cylinder, pushes the bottom plate to move upward, and the return spring receives the reverse force after elastic deformation to assist the push bottom plate to reset.

附图说明Description of drawings

图1为本发明提出的一种高收率环酸合成方法的整体结构示意图;Fig. 1 is the overall structural representation of a kind of high-yield cyclic acid synthesis method proposed by the present invention;

图2为本发明提出的一种高收率环酸合成方法的回气组件结构示意图;Fig. 2 is the structural representation of the gas return component of a kind of high-yield cyclic acid synthesis method proposed by the present invention;

图3为本发明提出的一种高收率环酸合成方法的气环结构示意图;Fig. 3 is the gas ring structure schematic diagram of a kind of high-yield cyclic acid synthesis method proposed by the present invention;

图4为本发明提出的一种高收率环酸合成方法的控温组件结构示意图;4 is a schematic structural diagram of a temperature control assembly of a high-yield cyclic acid synthesis method proposed by the present invention;

图5为本发明提出的一种高收率环酸合成方法的反应釜本体剖视结构示意图;Fig. 5 is the sectional structure schematic diagram of the reactor body of a kind of high-yield cyclic acid synthesis method proposed by the present invention;

图6为本发明提出的一种高收率环酸合成方法的搅拌组件结构示意图;6 is a schematic structural diagram of a stirring assembly of a high-yield cyclic acid synthesis method proposed by the present invention;

图7为本发明提出的一种高收率环酸合成方法的顶盖结构示意图;Fig. 7 is the top-cap structure schematic diagram of a kind of high-yield cyclic acid synthesis method proposed by the present invention;

图8为本发明提出的一种高收率环酸合成方法的调压组件结构示意图。8 is a schematic structural diagram of a pressure regulating assembly of a high-yield cyclic acid synthesis method proposed by the present invention.

图中:1、反应釜本体;2、回气座;3、气环;4、排气板;5、气孔;6、吸气管;7、进气槽;8、输气管;9、微型气泵;10、进气管;11、排气管;12、支座;13、支撑腿;14、顶盖;15、底盒;16、排料管;17、加热板;18、螺旋调温管;19、电热棒;20、进水管;21、出水管;22、机架;23、电动机;24、轴杆;25、进料口;26、六角轴座;27、支杆;28、弹簧底座;29、搅拌杆;30、溢气孔;31、气筒;32、气囊;33、气流控制阀;34、推压底板;35、内附座;36、复位弹簧。In the figure: 1. Reactor body; 2. Air return seat; 3. Air ring; 4. Exhaust plate; 5. Air hole; 6. Suction pipe; Air pump; 10. Intake pipe; 11. Exhaust pipe; 12. Support; 13. Support leg; 14. Top cover; 15. Bottom box; 16. Discharge pipe; 17. Heating plate; 18. Spiral thermostat ;19, electric heating rod; 20, water inlet pipe; 21, water outlet pipe; 22, frame; 23, electric motor; 24, shaft rod; 25, feed inlet; 26, hexagonal shaft seat; 27, strut; 28, spring Base; 29, stirring rod; 30, overflow hole; 31, air cylinder; 32, air bag; 33, air flow control valve; 34, push bottom plate; 35, attached seat; 36, return spring.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments.

一种高收率环酸合成方法,包括以下步骤:A high-yield cyclic acid synthesis method, comprising the following steps:

步骤一:将氨甲苯酸与纯水按照重量比1:5混合,在搅拌条件下缓慢加入浓硫酸,加热至预设温度,氨甲苯酸溶解,冷却结晶,过滤得到预处理后的氨甲苯酸,随后将质量分数5-7%的硫酸溶液、铂类催化剂和预处理后的氨甲苯酸按照重量比2:1:6的量从合成机构的进料口25加入反应釜本体1中,关闭反应釜本体1的进料口25,启动装置;Step 1: Mix aminotoluic acid and pure water in a weight ratio of 1:5, slowly add concentrated sulfuric acid under stirring conditions, heat to a preset temperature, dissolve aminotoluic acid, crystallize by cooling, and filter to obtain pretreated aminotoluic acid , then add 5-7% mass fraction of sulfuric acid solution, platinum-based catalyst and pretreated aminotoluic acid from the feed port 25 of the synthesis mechanism into the reactor body 1 according to the weight ratio of 2:1:6, and close the The feed port 25 of the reactor body 1, the startup device;

步骤二:加热板17通电后电热棒19对反应釜本体1内的溶液进行加热,待反应液温度达到预设温度后,电动机23带动轴杆24转动,搅拌组件对反应液进行混合搅拌;Step 2: After the heating plate 17 is energized, the electric heating rod 19 heats the solution in the reaction kettle body 1. After the temperature of the reaction solution reaches the preset temperature, the motor 23 drives the shaft 24 to rotate, and the stirring component mixes and stirs the reaction solution;

具体搅拌过程中,随着六角轴座26的转动,搅拌杆29受到内部反应液的反向作用力和轴杆24转动的驱动力,弹簧底座(28会发生晃动带动搅拌杆29振动,振动过程中搅拌杆29能够增加与反应液的接触效果,提高搅拌组件的整体搅拌混合效果;During the specific stirring process, with the rotation of the hexagonal shaft seat 26, the stirring rod 29 is subjected to the reverse force of the internal reaction solution and the driving force of the rotation of the shaft rod 24, and the spring base (28 will shake to drive the stirring rod 29 to vibrate, and the vibration process The middle stirring rod 29 can increase the contact effect with the reaction liquid and improve the overall stirring and mixing effect of the stirring assembly;

步骤三:从进气管10输送氢气至反应釜本体1的内部,输送定量氢气后关闭进气管10的阀门,制成加氢产物,然后再加入加氢产物重量比1:6的氢氧化钙,继续反应处理;Step 3: transport hydrogen from the inlet pipe 10 to the interior of the reactor body 1, close the valve of the inlet pipe 10 after transporting a certain amount of hydrogen to make a hydrogenated product, and then add calcium hydroxide with a weight ratio of 1:6 of the hydrogenated product, continue reaction processing;

氢气输送过程,氢气进入回气座2并从气孔5中喷出,直接作用在反应溶液中,氢气在反应液中形成气泡,增加了气体与反应液之间的接触效果,提高催化氢化效果,微型气泵9工作利用吸气管6和进气槽7对反应釜本体1的内部进行吸气操作,并通过输气管8进入回气座2内,从气孔5喷出,循环如此提高氢气与反应液的接触效果,反应结束后打开排气管11阀门排出反应釜内部的气体,随后将反应后的溶液排出进行后续的转位反应;During the hydrogen delivery process, the hydrogen gas enters the return gas seat 2 and is ejected from the air hole 5, and acts directly on the reaction solution. The hydrogen gas forms bubbles in the reaction solution, which increases the contact effect between the gas and the reaction solution and improves the catalytic hydrogenation effect. The micro air pump 9 works by using the air suction pipe 6 and the air inlet groove 7 to inhale the inside of the reactor body 1, and enters the air return seat 2 through the air delivery pipe 8, and ejects from the air hole 5, and the circulation improves the hydrogen and the reaction in this way. The contact effect of the liquid, after the reaction ends, open the valve of the exhaust pipe 11 to discharge the gas inside the reactor, and then discharge the reacted solution for subsequent transposition reaction;

步骤四:催化氢化反应期间,反应釜内部通入氢气,内部的压强会增大,催化氢化反应的效果会降低,而调压组件能够改变反应釜本体1内部的压强,当氢气通入后,气流控制阀33会进行排气操作,将气囊32中的气体向外排出,气囊32于气筒31中收缩体积,推压底板34向上移动,复位弹簧36受到弹性形变后的反向作用力来辅助推压底板36复位,进而完成高收率的环酸合成;如图1、图2和图3所示,包括反应釜本体1,反应釜本体1的内部设置有回气组件,且回气组件包括回气座2和气环3,回气座2的一侧外壁与反应釜本体1的内壁之间通过螺栓连接,且回气座2上设置有排气板4,排气板4上呈圆周等距开设有多个气孔5,气环3位于回气座2的上方,气环3与反应釜本体1的内壁之间通过螺栓连接,且气环3上开设有多个呈圆周等距的圆孔,圆孔的内壁通过螺栓连接有吸气管6,吸气管6的另一端均通过螺栓连接有进气槽7,气环3与回气座2之间通过螺栓连接有两个输气管8,且两个输气管8上均设置有微型气泵9,氢气输送过程,氢气进入回气座2并从气孔5中喷出,直接作用在反应溶液中,氢气在反应液中形成气泡,进一步增加了气体与反应液之间的接触效果,从而提高催化氢化效果。Step 4: During the catalytic hydrogenation reaction, hydrogen is introduced into the reactor, the internal pressure will increase, the effect of the catalytic hydrogenation reaction will be reduced, and the pressure regulating component can change the pressure inside the reactor body 1. When the hydrogen is introduced, The air flow control valve 33 will perform an exhaust operation to discharge the gas in the air bag 32 to the outside. The air bag 32 shrinks in the air cylinder 31 and pushes the bottom plate 34 to move upward. The return spring 36 is assisted by the reverse force after elastic deformation. Push the bottom plate 36 to reset, and then complete the high-yield cyclic acid synthesis; as shown in Figure 1, Figure 2 and Figure 3, including the reactor body 1, the interior of the reactor body 1 is provided with a gas return component, and the gas return component Including the gas return seat 2 and the gas ring 3, the outer wall of one side of the gas return seat 2 and the inner wall of the reactor body 1 are connected by bolts, and the gas return seat 2 is provided with an exhaust plate 4, and the exhaust plate 4 is in the shape of a circle. There are a plurality of air holes 5 equidistantly, the air ring 3 is located above the air return seat 2, the air ring 3 and the inner wall of the reactor body 1 are connected by bolts, and the air ring 3 is provided with a plurality of equidistant circumferentially. A round hole, the inner wall of the round hole is connected with an air intake pipe 6 by bolts, the other end of the air intake pipe 6 is connected with an air intake groove 7 by bolts, and the air ring 3 and the air return seat 2 are connected by bolts. Gas pipe 8, and two gas transmission pipes 8 are provided with micro air pump 9. During the hydrogen delivery process, hydrogen gas enters the gas return seat 2 and is ejected from the air hole 5, and directly acts on the reaction solution, and the hydrogen gas forms bubbles in the reaction solution, The contact effect between the gas and the reaction liquid is further increased, thereby improving the catalytic hydrogenation effect.

进一步的,如图2所示,回气座2上通过螺栓连接有进气管10,进气管10的另一端穿过反应釜本体1与外界的气管通过螺栓连接,且反应釜本体1上开设有圆孔,圆孔位于气环3的上方,圆孔的内壁通过螺栓连接有排气管11;反应釜本体1的外壁通过螺栓连接有三个呈圆周等距的支座12,支座12上均通过螺栓连接有支撑腿13,且反应釜本体1的上方设置有顶盖14,反应釜本体1的下方设置有底盒15,底盒15上开设有漏孔,漏孔的内壁通过螺栓连接有排料管16。Further, as shown in FIG. 2 , the air return seat 2 is connected with an air inlet pipe 10 by bolts, and the other end of the air inlet pipe 10 passes through the reactor body 1 and is connected with the outside air pipe by bolts, and the reactor body 1 is provided with The circular hole is located above the gas ring 3, and the inner wall of the circular hole is connected with an exhaust pipe 11 by bolts; The support legs 13 are connected by bolts, a top cover 14 is provided above the reactor body 1, and a bottom box 15 is provided below the reactor body 1. The bottom box 15 is provided with a leak hole, and the inner wall of the leak hole is connected by bolts. Discharge pipe 16.

更进一步的,如图1和图4所示,反应釜本体1的内部设置有控温组件,控温组件位于回气座2的下方,控温组件包括加热板17和螺旋调温管18,加热板17与反应釜本体1的内壁之间通过螺栓连接,加热板17上设置有多个圆周等距的电热棒19,且反应釜本体1上开设有两个圆孔,两个圆孔的内壁分别通过螺栓连接有进水管20和出水管21,进水管20和出水管21分别与螺旋调温管18的两端通过螺栓连接,加热板17通电后电热棒19对反应釜本体1内的溶液进行加热,使得待反应液温度达到预设温度,满足反应所需的条件,螺旋调温管18内通入调温液体(水),随着反应时间的加长或者加热板17加热过度,反应液的温度超过预设值,将水从进水管20输入,出水管21送出,对反应液进行降温操作,避免温度过高影响反应的整体进程。Further, as shown in FIG. 1 and FIG. 4 , the inside of the reactor body 1 is provided with a temperature control assembly, the temperature control assembly is located below the return air seat 2, and the temperature control assembly includes a heating plate 17 and a spiral temperature adjustment pipe 18, The heating plate 17 and the inner wall of the reactor body 1 are connected by bolts. The heating plate 17 is provided with a plurality of electric heating rods 19 with equidistant circumferences, and the reactor body 1 is provided with two circular holes. The inner wall is respectively connected with the water inlet pipe 20 and the water outlet pipe 21 by bolts, and the water inlet pipe 20 and the water outlet pipe 21 are respectively connected with the two ends of the spiral temperature regulating pipe 18 by bolts. The solution is heated so that the temperature of the liquid to be reacted reaches the preset temperature and meets the conditions required for the reaction. The temperature-adjusting liquid (water) is introduced into the spiral temperature-adjusting tube 18. As the reaction time increases or the heating plate 17 is overheated, the reaction When the temperature of the liquid exceeds the preset value, water is input from the water inlet pipe 20 and sent out from the water outlet pipe 21, and the reaction liquid is cooled down to avoid the overheating affecting the overall process of the reaction.

更进一步的,如图5和图6所示,顶盖14的上侧外壁通过螺栓连接有机架22,机架22的内壁通过螺栓连接有电动机23,电动机23的输出端通过联轴器连接有轴杆24,且轴杆24的另一端穿过顶盖14,轴杆24的外部设置有搅拌组件,顶盖14上开设有进料口25;搅拌组件包括六角轴座26和多个支杆27,六角轴座26上开设有六角凹槽,六角凹槽的内壁与轴杆24的外壁之间通过螺栓连接,且多个支杆27与六角轴座26之间通过螺栓连接,多个支杆27呈圆周等距分布;多个支杆27上均开设有三个等距的圆孔,三个圆孔的内壁均通过螺栓连接有弹簧底座28,且弹簧底座28的顶端均通过螺栓连接有搅拌杆29,搅拌过程中,随着六角轴座26的转动,搅拌杆29受到内部反应液的反向作用力和轴杆24转动的驱动力,弹簧底座28会发生晃动带动搅拌杆29振动,振动过程中搅拌杆29能够增加与反应液的接触效果,从而提高搅拌组件的整体搅拌混合效果。Further, as shown in FIG. 5 and FIG. 6 , the upper outer wall of the top cover 14 is connected with a frame 22 by bolts, the inner wall of the frame 22 is connected with a motor 23 by bolts, and the output end of the motor 23 is connected by a coupling. There is a shaft rod 24, and the other end of the shaft rod 24 passes through the top cover 14. A stirring assembly is provided on the outside of the shaft rod 24, and a feeding port 25 is opened on the top cover 14; the stirring assembly includes a hexagonal shaft seat 26 and a plurality of supports The rod 27 and the hexagonal shaft seat 26 are provided with a hexagonal groove, the inner wall of the hexagonal groove and the outer wall of the shaft rod 24 are connected by bolts, and the plurality of struts 27 and the hexagonal shaft seat 26 are connected by bolts, and many The struts 27 are distributed at equal distances around the circumference; the multiple struts 27 are provided with three equidistant circular holes, the inner walls of the three circular holes are all connected with a spring base 28 by bolts, and the tops of the spring bases 28 are all connected by bolts There is a stirring rod 29. During the stirring process, with the rotation of the hexagonal shaft seat 26, the stirring rod 29 is subjected to the reverse force of the internal reaction liquid and the driving force of the rotation of the shaft rod 24, and the spring base 28 will shake and drive the stirring rod 29 to vibrate. , during the vibration process, the stirring rod 29 can increase the contact effect with the reaction liquid, thereby improving the overall stirring and mixing effect of the stirring assembly.

更进一步的,如图7和图8所示,顶盖14上开设有两个对称的溢气孔30,且两个溢气孔30的内部均设置有调压组件;调压组件包括气筒31和气囊32,气筒31的外壁与溢气孔30的内壁之间通过螺栓连接,且气囊32位于气筒31的内部,气筒31的顶部通过螺栓连接有气流控制阀33,气流控制阀33与气囊32之间通过短管连接;气囊32的内部设置有推压底板34,且气囊32的顶部内壁通过螺栓连接有内附座35,内附座35的下侧外壁通过螺栓连接有复位弹簧36,复位弹簧36的另一端与推压底板34之间通过螺栓连接,催化氢化反应期间,由于反应釜内部通入氢气,其内部的压强会增大,从而催化氢化反应的效果会降低(气压增大后氢气的溶解度降低),而调压组件能够改变反应釜本体1内部的压强,当氢气通入后,气流控制阀33会进行排气操作,将气囊32中的气体向外排出(初始时气囊32中充入外界的空气使其膨胀),气囊32于气筒31中收缩体积,推压底板34向上移动,复位弹簧36受到弹性形变后的反向作用力来辅助推压底板34复位。Further, as shown in FIG. 7 and FIG. 8 , the top cover 14 is provided with two symmetrical overflow holes 30, and the inside of the two overflow holes 30 are provided with pressure regulating components; the pressure regulating components include an air cylinder 31 and an air bag. 32. The outer wall of the air cylinder 31 is connected with the inner wall of the overflow hole 30 by bolts, and the air bag 32 is located inside the air cylinder 31. The top of the air cylinder 31 is connected with an air flow control valve 33 by bolts, and the air flow control valve 33 and the air bag 32 pass through. Short pipe connection; the inside of the airbag 32 is provided with a pushing bottom plate 34, and the top inner wall of the airbag 32 is connected with an inner attachment seat 35 by bolts, and the lower side outer wall of the inner attachment seat 35 is connected with a return spring 36 by bolts. The other end is connected with the pushing bottom plate 34 by bolts. During the catalytic hydrogenation reaction, due to the introduction of hydrogen into the reactor, the internal pressure will increase, so that the effect of the catalytic hydrogenation reaction will be reduced (the solubility of hydrogen after the pressure increases). lower), and the pressure regulating component can change the pressure inside the reactor body 1. When the hydrogen gas is introduced, the airflow control valve 33 will perform an exhaust operation to discharge the gas in the air bag 32 to the outside (initially, the air bag 32 is filled with The outside air makes it expand), the air bag 32 shrinks in the air cylinder 31, pushes the bottom plate 34 to move upward, and the return spring 36 receives the reverse force after elastic deformation to assist the push bottom plate 34 to reset.

以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited to this. The equivalent replacement or change of the inventive concept thereof shall be included within the protection scope of the present invention.

Claims (10)

1. A high-yield cyclic acid synthesis method is characterized by comprising the following steps:
the method comprises the following steps: mixing aminomethylbenzoic acid and pure water according to a weight ratio of 1:5, slowly adding concentrated sulfuric acid under stirring, heating to a preset temperature, dissolving the aminomethylbenzoic acid, cooling for crystallization, filtering to obtain pretreated aminomethylbenzoic acid, then adding a sulfuric acid solution with a mass fraction of 5-7%, a platinum catalyst and the pretreated aminomethylbenzoic acid into a reaction kettle body (1) from a feed inlet (25) of a synthesis mechanism according to a weight ratio of 2:1:6, closing the feed inlet (25) of the reaction kettle body (1), and starting a device;
step two: after the heating plate (17) is electrified, the electric heating rod (19) heats the solution in the reaction kettle body (1), after the temperature of the reaction liquid reaches a preset temperature, the motor (23) drives the shaft lever (24) to rotate, and the stirring assembly mixes and stirs the reaction liquid;
in the concrete stirring process, along with the rotation of the hexagonal shaft seat (26), the stirring rod (29) receives the reverse acting force of the internal reaction liquid and the driving force of the rotation of the shaft lever (24), the spring base (28) can shake to drive the stirring rod (29) to vibrate, the stirring rod (29) can increase the contact effect with the reaction liquid in the vibration process, and the overall stirring and mixing effect of the stirring assembly is improved;
step three: conveying hydrogen from an air inlet pipe (10) to the interior of the reaction kettle body (1), closing a valve of the air inlet pipe (10) after conveying quantitative hydrogen to prepare a hydrogenation product, then adding calcium hydroxide with the weight ratio of the hydrogenation product being 1:6, and continuing reaction treatment;
during the hydrogen conveying process, hydrogen enters the gas return seat (2) and is sprayed out of the gas holes (5) to directly act on reaction solution, the hydrogen forms bubbles in the reaction solution, the contact effect between the gas and the reaction solution is increased, the catalytic hydrogenation effect is improved, the miniature gas pump (9) works by utilizing the gas suction pipe (6) and the gas inlet groove (7) to suck gas into the reaction kettle body (1), the gas enters the gas return seat (2) through the gas conveying pipe (8), the hydrogen is sprayed out of the gas holes (5), the contact effect between the hydrogen and the reaction solution is circularly improved, after the reaction is finished, the valve of the exhaust pipe (11) is opened to exhaust the gas in the reaction kettle, and then the reacted solution is exhausted to perform subsequent transposition reaction;
step four: during the catalytic hydrogenation reaction, inside the reation kettle lets in hydrogen, inside pressure can increase, catalytic hydrogenation reaction's effect can reduce, and the pressure regulating subassembly can change the inside pressure of reation kettle body (1), after hydrogen lets in, air current control valve (33) can carry out the exhaust operation, outwards discharge the gas in gasbag (32), gasbag (32) shrink volume in inflator (31), bulldoze bottom plate (34) rebound, reset spring (36) receive the reverse effort behind the elastic deformation to assist and bulldoze bottom plate (36) and reset, and then accomplish high yield's cyclic acid synthesis.
2. The method for synthesizing the high-yield naphthenic acid according to claim 1, wherein the synthesis mechanism comprises a reaction kettle body (1), a gas return assembly is arranged inside the reaction kettle body (1), the gas return assembly comprises a gas return seat (2) and a gas ring (3), the outer wall of one side of the gas return seat (2) is fixedly connected with the inner wall of the reaction kettle body (1), an exhaust plate (4) is arranged on the gas return seat (2), a plurality of gas holes (5) are formed in the exhaust plate (4) at equal intervals on the circumference, the gas ring (3) is positioned above the gas return seat (2), the gas ring (3) is fixedly connected with the inner wall of the reaction kettle body (1), a plurality of circular holes at equal intervals on the circumference are formed in the gas ring (3), a gas suction pipe (6) is fixedly connected with the inner wall of the circular hole, and a gas inlet groove (7) is fixedly connected with the other end of the gas suction pipe (6), two air pipes (8) are fixedly connected between the air ring (3) and the air return seat (2), and a micro air pump (9) is arranged on each of the two air pipes (8).
3. The method for synthesizing the cyclic acid with high yield according to claim 2, wherein the gas inlet pipe (10) is fixedly connected to the gas return base (2), the other end of the gas inlet pipe (10) penetrates through the reaction kettle body (1) to be fixedly connected with an external gas pipe, a circular hole is formed in the reaction kettle body (1), the circular hole is located above the gas ring (3), and an exhaust pipe (11) is fixedly connected to the inner wall of the circular hole.
4. The method for synthesizing the high-yield cyclic acid according to claim 3, wherein three supports (12) with equal intervals in the circumference are fixedly connected to the outer wall of the reaction kettle body (1), the supports (12) are all fixedly connected with supporting legs (13), a top cover (14) is arranged above the reaction kettle body (1), a bottom box (15) is arranged below the reaction kettle body (1), a leakage hole is formed in the bottom box (15), and a discharge pipe (16) is fixedly connected to the inner wall of the leakage hole.
5. The method for synthesizing the high-yield naphthenic acid according to claim 4, wherein a temperature control assembly is arranged inside the reaction kettle body (1), the temperature control assembly is located below the gas return seat (2), the temperature control assembly comprises a heating plate (17) and a spiral temperature adjusting pipe (18), the heating plate (17) is fixedly connected with the inner wall of the reaction kettle body (1), a plurality of electric heating rods (19) with equal circumferential distances are arranged on the heating plate (17), two round holes are formed in the reaction kettle body (1), the inner walls of the two round holes are respectively and fixedly connected with a water inlet pipe (20) and a water outlet pipe (21), and the water inlet pipe (20) and the water outlet pipe (21) are respectively and fixedly connected with two ends of the spiral temperature adjusting pipe (18).
6. The method for synthesizing the high-yield naphthenic acid according to claim 2, wherein a rack (22) is fixedly connected to the outer wall of the upper side of the top cover (14), a motor (23) is fixedly connected to the inner wall of the rack (22), the output end of the motor (23) is connected with a shaft rod (24) through a coupling, the other end of the shaft rod (24) penetrates through the top cover (14), a stirring assembly is arranged outside the shaft rod (24), and a feeding hole (25) is formed in the top cover (14).
7. The method for synthesizing high-yield naphthenic acid according to claim 6, wherein the stirring assembly comprises a hexagonal shaft seat (26) and a plurality of struts (27), the hexagonal shaft seat (26) is provided with a hexagonal groove, the inner wall of the hexagonal groove is fixedly connected with the outer wall of the shaft rod (24), the plurality of struts (27) are fixedly connected with the hexagonal shaft seat (26), and the plurality of struts (27) are circumferentially distributed at equal intervals.
8. The method for synthesizing the cyclic acid with high yield according to claim 7, wherein three circular holes with equal distance are formed on the plurality of the supporting rods (27), the inner walls of the three circular holes are fixedly connected with spring bases (28), and the top ends of the spring bases (28) are fixedly connected with stirring rods (29).
9. The method for synthesizing the cyclic acid with high yield according to claim 8, wherein the top cover (14) is provided with two symmetrical air overflow holes (30), and pressure regulating components are arranged inside the two air overflow holes (30).
10. The method for synthesizing the cyclic acid with high yield according to claim 9, wherein the pressure regulating assembly comprises a gas cylinder (31) and a gas bag (32), the outer wall of the gas cylinder (31) is fixedly connected with the inner wall of the gas overflow hole (30), the gas bag (32) is positioned inside the gas cylinder (31), the top of the gas cylinder (31) is fixedly connected with a gas flow control valve (33), and the gas flow control valve (33) is connected with the gas bag (32) through a short pipe; the inner part of the air bag (32) is provided with a pushing and pressing bottom plate (34), an inner attached seat (35) is fixedly connected to the inner wall of the top of the air bag (32), a return spring (36) is fixedly connected to the outer wall of the lower side of the inner attached seat (35), and the other end of the return spring (36) is fixedly connected with the pushing and pressing bottom plate (34).
CN202210488611.XA 2022-05-06 2022-05-06 A kind of high-yield cyclic acid synthesis method Pending CN114671773A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116393019A (en) * 2023-05-29 2023-07-07 青州金昊新材料有限公司 Circulation cooling type liquid chemical raw material mixing equipment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116393019A (en) * 2023-05-29 2023-07-07 青州金昊新材料有限公司 Circulation cooling type liquid chemical raw material mixing equipment
CN116393019B (en) * 2023-05-29 2023-08-15 青州金昊新材料有限公司 Circulation cooling type liquid chemical raw material mixing equipment

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Application publication date: 20220628