Industrial method for purifying tert-butyl peroxybenzoate

文档序号:1793098 发布日期:2021-11-05 浏览:28次 中文

阅读说明:本技术 一种用于提纯过氧化苯甲酸叔丁酯的工业方法 (Industrial method for purifying tert-butyl peroxybenzoate ) 是由 茆金年 徐立 高德亮 于 2021-08-11 设计创作,主要内容包括:本发明公开了一种用于提纯过氧化苯甲酸叔丁酯的工业方法,S1.反应釜温度为15-25℃,向反应釜内加入叔丁基过氧化氢和活性剂搅拌,再将氢氧化钠溶液倒入反应釜中混合搅拌,获得第一混合液,对第一混合液进行萃取析出钠盐,获得钠盐和滤液,萃取液为乙醇;S2.向所述钠盐中加入-3℃的纯净水缓慢搅拌,获得糊状混合物;S3.向苯甲酰氯内添加催化剂搅拌,获得第二混合液,再通过冷凝管滴入至糊状混合物中搅拌,获得粗品过氧化苯甲酸叔丁酯;S4.将所述粗品过氧化苯甲酸叔丁酯通过碳酸钠洗涤分离,硫酸镁溶液洗涤一次,干燥获得过氧化苯甲酸叔丁酯。本发明在制备过氧化苯甲酸叔丁酯中,减少叔丁基过氧化氢的含量,加快叔丁基过氧化氢和氢氧化钠的反应。(The invention discloses an industrial method for purifying tert-butyl peroxybenzoate, which comprises the following steps of S1, controlling the temperature of a reaction kettle to be 15-25 ℃, adding tert-butyl hydroperoxide and an active agent into the reaction kettle, stirring, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring to obtain a first mixed solution, extracting the first mixed solution to separate out sodium salt, obtaining sodium salt and filtrate, wherein the extract is ethanol; s2, adding purified water at the temperature of-3 ℃ into the sodium salt, and slowly stirring to obtain a pasty mixture; s3, adding a catalyst into benzoyl chloride, stirring to obtain a second mixed solution, and then, dropwise adding the second mixed solution into the pasty mixture through a condensation tube, and stirring to obtain a crude tert-butyl peroxybenzoate; and S4, washing and separating the crude tert-butyl peroxybenzoate by using sodium carbonate, washing once by using magnesium sulfate solution, and drying to obtain tert-butyl peroxybenzoate. The invention reduces the content of tert-butyl hydroperoxide and accelerates the reaction of tert-butyl hydroperoxide and sodium hydroxide in the preparation of tert-butyl peroxybenzoate.)

1. An industrial process for purifying tert-butyl peroxybenzoate, characterized in that it comprises the following steps:

s1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle at the temperature of 15-25 ℃, stirring for 5-9min, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring, wherein the mass ratio of the active agent to the tert-butyl hydroperoxide to the sodium hydroxide solution is 1:35-55:18-29, stirring for 35-55min to obtain a first mixed solution, controlling the pH value of the first mixed solution to be 10-14, extracting the first mixed solution to separate out sodium salt to obtain sodium salt and filtrate, wherein the mass ratio of the extract to the mixed solution is 1: 5;

s2, adding purified water at the temperature of-3 ℃ into the sodium salt, slowly stirring, and stirring for 20-30min to obtain a pasty mixture;

s3, taking a plurality of parts of benzoyl chloride, adding a catalyst into the benzoyl chloride, stirring for 4-9min to obtain a second mixed solution, wherein the mass ratio of the benzoyl chloride to the catalyst is 12-15:1, dripping the second mixed solution into the pasty mixture through a condensation pipe, stirring, standing and separating after stirring for a preset time to obtain a crude tert-butyl peroxybenzoate;

and S4, washing and separating the crude tert-butyl peroxybenzoate by sodium carbonate, washing once by magnesium sulfate solution, finally putting into a storage tank, and drying to obtain tert-butyl peroxybenzoate.

2. The industrial process for purifying tert-butyl peroxybenzoate according to claim 1, characterized in that said active agents comprise styrene, sodium alkylbenzenesulfonate and saponin in a mass ratio of 1:0.5: 1.5.

3. The industrial process for purifying tert-butyl peroxybenzoate according to claim 1, wherein said catalyst is potassium permanganate or chlorate.

4. The industrial process for purifying tert-butyl peroxybenzoate according to claim 2, wherein in said S2, purified water is used at a flow rate of 0.2cm3Stirring with sodium salt at a speed of 10-15 rpm.

5. The industrial method for purifying tert-butyl peroxybenzoate according to claim 4, wherein in S3, the dropping speed of the second mixed solution is 20-30 drops/min, and the stirring time is 70-90 min.

6. The industrial method for purifying tert-butyl peroxybenzoate according to claim 1, characterized in that said reaction vessel comprises a reaction device (1), a placing device (2) and a control device (3), said placing device (2) is connected with the upper end of said reaction device (1), a support frame (4) is connected with said placing device (2), said control device (3) is connected with said support frame (4), a switch (5) for controlling the opening/closing of said reaction device (1) is arranged on said placing device (2);

reaction unit (1) includes reaction box (110), inner bag (120) and refrigeration passageway (130), be provided with inner bag (120) in reaction box (110), reaction box (110) inner wall with be provided with the refrigeration passageway between inner bag (120), inner bag (120) are used for tert-butyl hydroperoxide and the container that the sodium hydroxide solution was used for reacting, the refrigeration passageway is used for letting in air conditioning, guarantees to keep constant temperature low temperature in inner bag (120), be provided with stirring piece (6) in reaction box (110).

7. The industrial process for purifying tert-butyl peroxybenzoate according to claim 6, characterized in that said placing means (2) comprises a first containing tank (210) and a second containing tank (220), said tert-butyl hydroperoxide and sodium hydroxide solution being respectively filled in said first containing tank (210) and said second containing tank (220).

8. The industrial process for purifying tert-butyl peroxybenzoate according to claim 6, characterized in that said control means (3) comprise a screw (310) and two sets of lifters (320), said switches comprising a first switch (510) and a second switch (520), respectively located directly below the two sets of lifters (320).

9. The industrial method for purifying tert-butyl peroxybenzoate according to claim 8, wherein said screw (310) is fixedly connected to the supporting frame (4), said screw (310) is connected with a nut (330) adapted thereto, and one end of said lifting member (320) is connected with the nut (330).

10. The industrial method for purifying tert-butyl peroxybenzoate according to claim 9, wherein said lifting member (320) comprises a roller (320 a), an iron wire (320 b) and a fixed block (320 c), said iron wire (320 b) is wound around the roller (320 a), said roller (320 a) is fixedly connected to the supporting frame (4), one end of said iron wire (320 b) is connected to the nut (330), and the other end is connected to the fixed block (320 c), and said two sets of lifting members (320) are arranged in mirror image.

Technical Field

The invention relates to the technical field of tert-butyl peroxybenzoate, in particular to an industrial method for purifying tert-butyl peroxybenzoate.

Background

Tert-butyl peroxybenzoate is an organic compound of formula C11H14O3, a colorless to yellowish liquid. Has a slight aromatic odor. Is insoluble in water and soluble in organic solvent. Tert-butyl peroxybenzoate is widely used as an initiator in polymerization processes such as ethylene, styrene, propylene, vinyl acetate, diallyl phthalate, and isobutylene. In the unsaturated polyester curing process, the unsaturated polyester curing agent is widely applied to forming processes such as SMC, BMC, DMC drawing agent and the like, and simultaneously can also be applied to a two-component curing system formed by MEPK, BPO or TBPO and the like with higher activity. Storing in a cool and ventilated storehouse. Keep away from the fire species, heat source, prevent the direct projection of sunshine. The temperature of the storage is not more than 30 ℃. And (7) packaging and sealing. Should be stored separately from the reducing agent and alkali, and should not be stored in a mixed manner. And preparing fire-fighting equipment of corresponding varieties and quantity. The reservoir should be provided with a suitable material to contain the leakage. Vibrations, impacts and friction are prohibited.

In the preparation of tert-butyl peroxybenzoate, the conversion rate is low due to the fact that impurities are more, and in the preparation of tert-butyl peroxybenzoate, if the dosage of tert-butyl hydroperoxide is too much, the dosage of tert-butyl hydroperoxide can cause too much tert-butyl hydroperoxide, repeated washing is needed in the final purification, and in the reaction process, the conversion rate is influenced by the temperature.

Disclosure of Invention

In order to solve the above-mentioned defects of the prior art, the invention provides an industrial method for purifying tert-butyl peroxybenzoate.

In order to solve the technical problems, the invention adopts the following technical scheme: an industrial process for purifying tert-butyl peroxybenzoate comprising the steps of:

s1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle at the temperature of 15-25 ℃, stirring for 5-9min, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring, wherein the mass ratio of the active agent to the tert-butyl hydroperoxide to the sodium hydroxide solution is 1:35-55:18-29, stirring for 35-55min to obtain a first mixed solution, controlling the pH value of the first mixed solution to be 10-14, and extracting the first mixed solution to separate out sodium salt to obtain sodium salt and filtrate;

s2, adding purified water at the temperature of-3 ℃ into the sodium salt, slowly stirring, and stirring for 20-30min to obtain a pasty mixture;

s3, taking a plurality of parts of benzoyl chloride, adding a catalyst into the benzoyl chloride, stirring for 4-9min to obtain a second mixed solution, wherein the mass ratio of the benzoyl chloride to the catalyst is 12-15:1, dripping the second mixed solution into the pasty mixture through a condenser pipe, stirring, standing and separating for a preset time, obtaining a crude tert-butyl peroxybenzoate, and reacting a sodium salt and the benzoyl chloride at a low temperature;

and S4, washing and separating the crude tert-butyl peroxybenzoate by sodium carbonate, washing once by magnesium sulfate solution, finally putting into a storage tank, and drying to obtain tert-butyl peroxybenzoate.

Preferably, the active agent comprises styrene, sodium alkyl benzene sulfonate and saponin in a mass ratio of 1:0.5: 1.5.

The styrene is insoluble in water, the styrene can be used as a catalyst to accelerate the reaction of the tert-butyl hydroperoxide and the sodium hydroxide, so that the reaction of the tert-butyl hydroperoxide and the sodium hydroxide is more complete, the saponin can reduce the surface tension of the liquid, the sodium alkyl benzene sulfonate has a dispersing effect, is an anionic surfactant, is matched with the saponin, and accelerates the reaction of the tert-butyl hydroperoxide and the sodium hydroxide, thereby reducing the content of the tert-butyl hydroperoxide.

Preferably, the catalyst is potassium permanganate or chlorate, the potassium permanganate or chlorate can accelerate the replacement of chloride ions on benzene by hydrogen ions, and the potassium permanganate or chlorate is dissolved in water and can be separated by utilizing the characteristic of water solubility.

Preferably, in the S2, the purified water has a flow rate of 0.2cm3Stirring with sodium salt at a speed of 10-15 rpm.

Preferably, in S3, the dropping speed of the second mixed solution is 20 to 30 drops/min, and the stirring time is 70 to 90 min.

Preferably, the reaction kettle comprises a reaction device, a placing device and a control device, the placing device is connected with the upper end of the reaction device, a support frame is connected onto the placing device, the control device is connected with the support frame, and a switch for controlling the reaction device to be turned on/off is arranged on the placing device;

the reaction device comprises a reaction box, an inner container and a refrigeration channel, wherein the inner container is arranged in the reaction box, the refrigeration channel is arranged between the inner wall of the reaction box and the inner container, the inner container is used for a container for reacting tert-butyl hydroperoxide and sodium hydroxide solution, the refrigeration channel is used for introducing cold air to ensure that the inner container is kept at constant temperature and low temperature, and a stirring piece is arranged in the reaction box;

the tert-butyl hydroperoxide is decomposed when heated, the tert-butyl hydroperoxide reacts with the sodium hydroxide to generate sodium salt and water, and when the water is generated in the reaction, the sodium hydroxide releases heat when contacting with the water to improve the temperature of the reaction environment, so that the structure of the tert-butyl hydroperoxide is damaged, the refrigeration channel is used for introducing cold air to ensure that the inner container is kept at a constant temperature and a low temperature, the temperature of the tert-butyl hydroperoxide and the sodium hydroxide during the reaction is controlled, the consumption of the tert-butyl hydroperoxide is reduced, and the content of the tert-butyl peroxybenzoate is increased.

Preferably, the placing device comprises a first containing box and a second containing box, and the tert-butyl hydroperoxide and the sodium hydroxide solution are respectively filled in the first containing box and the second containing box.

Preferably, the control device comprises a screw rod and two groups of lifting pieces, the switches comprise a first switch and a second switch which are respectively positioned under the two groups of lifting pieces, the screw rod is fixedly connected to the support frame, the screw rod is connected with nuts matched with the screw rod, and one end of each lifting piece is connected with the nut.

Preferably, the lifting part comprises a roller, an iron wire and a fixed block, the iron wire is wound on the roller and is connected with the roller, the roller is fixedly connected onto the support frame, one end of the iron wire is connected with a nut, the other end of the iron wire is connected with the fixed block, and the two groups of lifting parts are arranged in a mirror mode.

Compared with the prior art, the invention has the beneficial effects that: the invention reduces the content of tert-butyl hydroperoxide and accelerates the reaction of tert-butyl hydroperoxide and sodium hydroxide in the preparation of tert-butyl peroxybenzoate.

Drawings

FIG. 1 is a graph showing the reaction rate of t-butyl hydroperoxide and sodium hydroxide according to the present invention.

FIG. 2 is a schematic view of the structure of the reaction vessel of the present invention.

Fig. 3 is a schematic structural diagram of the control device.

The labels in the figure are: the reaction device comprises a reaction device 1, a reaction box 110, a liner 120, a refrigeration channel 130, a placing device 2, a first accommodating box 210, a second accommodating box 220, a control device 3, a lead screw 310, a lifting piece 320, a roller 320a, an iron wire 320b, a fixed block 320c, a nut 330, a support frame 4, a switch 5, a first switch 510, a second switch 520 and a stirring piece 6.

Detailed Description

The invention is described in detail below with reference to the figures and examples.

Example 1

The invention provides an industrial method for purifying tert-butyl peroxybenzoate, which comprises the following steps:

s1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle at the temperature of 15 ℃, stirring for 5min, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring, wherein the mass ratio of the active agent to the tert-butyl hydroperoxide to the sodium hydroxide solution is 1: 35: 18, stirring an active agent comprising styrene, sodium alkyl benzene sulfonate and saponin in a mass ratio of 1:0.5:1.5 to obtain a first mixed solution, wherein the pH value of the first mixed solution is 10, the mixing and stirring time is 35min, extracting the first mixed solution to separate out sodium salt to obtain sodium salt and filtrate, wherein the extract is water or other solution insoluble in organic liquid, and the mass ratio of the extract to the mixed solution is 1: 5;

s2, adding purified water with the temperature of-3 ℃ into the sodium salt, wherein the flow rate of the purified water is 0.2cm3Stirring with sodium salt at a speed of 10 revolutions per minute to obtain a pasty mixture;

s3, taking a plurality of parts of benzoyl chloride, adding a catalyst into the benzoyl chloride, stirring for 4min to obtain a second mixed solution, wherein the catalyst is potassium permanganate, dripping the second mixed solution into the pasty mixture through a condenser pipe, stirring at the dripping speed of 20 drops/min for 70min, standing and separating to obtain a crude tert-butyl peroxybenzoate;

and S4, washing and separating the crude tert-butyl peroxybenzoate by sodium carbonate, washing once by magnesium sulfate solution, finally putting into a storage tank, and drying to obtain tert-butyl peroxybenzoate.

Example 2

An industrial process for purifying tert-butyl peroxybenzoate comprising the steps of:

s1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle at the temperature of 17 ℃, stirring for 7min, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring, wherein the mass ratio of the active agent to the tert-butyl hydroperoxide to the sodium hydroxide solution is 1: 42: 21, stirring an active agent comprising styrene, sodium alkyl benzene sulfonate and saponin in a mass ratio of 1:0.5:1.5 to obtain a first mixed solution, wherein the pH value of the first mixed solution is 12, the mixing and stirring time is 43min, extracting the first mixed solution to separate out sodium salt to obtain sodium salt and filtrate, wherein the extract is water or other solution insoluble in organic liquid, and the mass ratio of the extract to the mixed solution is 1: 5;

s2, adding purified water with the temperature of-3 ℃ into the sodium salt, wherein the flow rate of the purified water is 0.2cm3Stirring with sodium salt at a speed of 12 rpm to obtain a pasty mixture;

s3, taking a plurality of parts of benzoyl chloride, adding a catalyst into the benzoyl chloride, stirring for 6min to obtain a second mixed solution, wherein the catalyst is potassium permanganate, dripping the second mixed solution into the pasty mixture through a condensing tube, stirring at the dripping speed of 24 drops/min for 81min, and standing and separating to obtain a crude tert-butyl peroxybenzoate;

and S4, washing and separating the crude tert-butyl peroxybenzoate by sodium carbonate, washing once by magnesium sulfate solution, finally putting into a storage tank, and drying to obtain tert-butyl peroxybenzoate.

Example 3

An industrial process for purifying tert-butyl peroxybenzoate comprising the steps of:

s1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle at the temperature of 25 ℃, stirring for 9min, pouring a sodium hydroxide solution into the reaction kettle, mixing and stirring, wherein the mass ratio of the active agent to the tert-butyl hydroperoxide to the sodium hydroxide solution is 1: 55: 29, stirring the activator comprising styrene, sodium alkyl benzene sulfonate and saponin in a mass ratio of 1:0.5:1.5 to obtain a first mixed solution, extracting the first mixed solution to separate sodium salt to obtain sodium salt and filtrate, wherein the pH value of the first mixed solution is 14, and the mixing and stirring time is 55 min;

s2, adding purified water with the temperature of-3 ℃ into the sodium salt, wherein the flow rate of the purified water is 0.2cm3Stirring with sodium salt at a speed of 15 revolutions per minute to obtain a pasty mixture;

s3, taking a plurality of parts of benzoyl chloride, adding a catalyst into the benzoyl chloride, stirring for 4min to obtain a second mixed solution, wherein the catalyst is potassium permanganate, dripping the second mixed solution into the pasty mixture through a condenser pipe, stirring at the dripping speed of 30 drops/min for 90min, standing and separating to obtain a crude tert-butyl peroxybenzoate;

and S4, washing and separating the crude tert-butyl peroxybenzoate by sodium carbonate, washing once by magnesium sulfate solution, finally putting into a storage tank, and drying to obtain tert-butyl peroxybenzoate.

Comparative example 1

This comparative example is substantially the same as example 2 except that:

in step S1, the t-butyl hydroperoxide is not mixed with the active agent with agitation.

Comparative example 2

This comparative example is substantially the same as example 2 except that:

in step S1, the first mixed solution is not extracted and separated, the first mixed solution is directly filtered to obtain a residue, and in step S2, purified water is directly added to the residue.

Comparative example 3

This comparative example is substantially the same as example 2 except that:

in step S3, no catalyst was added to the benzoyl chloride.

Comparative example 4

This comparative example is substantially the same as example 2 except that:

in step S3, when the second mixed solution is dropped into the pasty mixture, a condenser tube is not used.

Comparative example 5

This comparative example is substantially the same as example 2 except that:

in step S1, the active agent includes sodium alkyl benzene sulfonate and saponin in a mass ratio of 0.5: 1.5.

Comparative example 6

This comparative example is substantially the same as example 2 except that:

in step S1, the activator is styrene.

The purity of t-butyl peroxybenzoate prepared by the preparation methods of examples 1 to 3 and comparative examples 1 to 7 was measured, and is shown in Table 1.

TABLE 1

Example 1 Example 2 Example 3 Comparative example 2 Comparative example 3 Comparative example 4
Tert-butyl peroxybenzoate content (%) 97.5% 98% 97% 94.8% 93.7% 94.1%
T-butyl hydroperoxide content (%) 1.8% 1.3% 2.3% 3.2% 1.3% 1.3%

Thus, example 2 is the best case, and the content of tert-butyl peroxybenzoate in comparative examples 2-4 is lower than that in examples 1-3.

In comparative example 2, ethanol is not used for extraction, and the characteristic that t-butyl hydroperoxide is slightly soluble in water is directly used for separating the mixed solution to obtain sodium salt, but t-butyl hydroperoxide dissolved in water cannot be separated, so that the impurity content of t-butyl hydroperoxide is increased.

In comparative example 3, no catalyst was added, so that the reaction between benzoyl chloride and sodium salt could not be completed, and the content of tert-butyl peroxybenzoate was reduced.

Comparative example 4 no benzoyl chloride was dropped into the pasty mixture through the condenser tube, but during the preparation of t-butyl peroxybenzoate, the temperature was first cooled through the condenser tube, and before the reaction, the temperature of benzoyl chloride was first lowered to accelerate the effective control of the reaction temperature, thereby accelerating the reaction rate of benzoyl chloride and sodium salt.

The reaction rates of t-butyl hydroperoxide and sodium hydroxide were observed using the preparation methods of example 2 and comparative examples 1 and 5 to 6, and specifically, see fig. 1;

the contents of t-butyl hydroperoxide after the reaction of t-butyl hydroperoxide and sodium hydroxide were observed by the preparation methods of example 2, comparative example 1 and comparative examples 5 to 6, and are specifically shown in table 2;

TABLE 2

Example 2 Comparative example 1 Comparative example 5 Comparative example 6
T-butyl hydroperoxide content (%) 2% 21% 10% 7%

As shown in fig. 1, the chemical reaction rate of comparative example 1 is significantly lower than that of example 2 without adding an active agent, and as shown in table 2, the active agent accelerates the chemical reaction rate and simultaneously enables the reaction between tert-butyl hydroperoxide and sodium hydroxide to be more complete, thereby reducing the impurities of tert-butyl hydroperoxide;

as shown in fig. 1, the chemical reaction rate of the comparative example 5 is higher than that of the comparative example 1 because styrene is not added in the activator, and as shown in table 2, the content of tert-butyl hydroperoxide is higher than that of the comparative example 1 because the tert-butyl hydroperoxide is higher than that of the comparative example 2, styrene is an excellent organic solvent and can accelerate the fusion of tert-butyl hydroperoxide and sodium hydroxide, and styrene can also be used as a catalyst to accelerate the reaction of tert-butyl hydroperoxide and sodium hydroxide;

in comparative example 6, sodium alkylbenzenesulfonate and saponin were not added as an active agent, but sodium alkylbenzenesulfonate had a dispersing action, and when the anionic surfactant was used in combination with the specificity of saponin, the reaction was accelerated while the fusion of t-butyl hydroperoxide and sodium hydroxide was accelerated, as shown in fig. 1, the chemical reaction rate of comparative example 6 was higher than that of comparative example 5, and as shown in table 2, the content of t-butyl hydroperoxide was higher than that of example 2 and lower than that of comparative example 5.

Example 4

As shown in fig. 2-3, the reaction kettle used in this embodiment includes a reaction device 1, a placing device 2 and a control device 3, the reaction device 1 includes a reaction box 110, an inner container 120 and a gas channel 130, the inner container 120 is disposed in the reaction box 110, a refrigeration channel is disposed between the inner wall of the reaction box 110 and the inner container 120, the inner container 120 is used for a container for reacting the t-butyl hydroperoxide and the sodium hydroxide solution, the refrigeration channel is used for introducing cold gas, a refrigerator can be placed in the refrigeration channel and also can be communicated with an external refrigerator to convey cold air to the refrigeration channel, so that the constant temperature and the low temperature can be continuously kept in the inner container 120, the temperature of the tert-butyl hydroperoxide and the sodium hydroxide during reaction can be controlled, the consumption of the tert-butyl hydroperoxide is reduced, thereby increasing the content of tert-butyl peroxybenzoate, a stirring piece 6 is arranged in the reaction box 110, and the stirring piece 6 is used for stirring tert-butyl hydroperoxide and sodium hydroxide;

the placing device 2 comprises a first containing box 210 and a second containing box 220, and is located right above the reaction box 110, tert-butyl hydroperoxide is filled in the first containing box 210, sodium hydroxide is filled in the second containing box 220, a first switch 510 for controlling the first containing box 210 to be opened/closed is arranged on the upper surface of the first containing box 210, a second switch 520 matched with the first containing box 220 to be opened/closed is arranged on the upper surface of the second containing box 220, it should be noted that the switches on the first containing box 210 and the second containing box 220 are independent switches, are not affected with each other, and can only control the corresponding containing box to be opened or closed, and are opened when the switches are touched, and are closed otherwise;

be connected with support frame 4 on placer 2, controlling means 3 is connected with support frame 4, controlling means 3 includes lead screw 310 and two sets of lifting member 320, two sets of lifting member 320 are located first switch 510 and second switch 520 directly over respectively, lifting member 320 is used for touching first switch 510 and second switch 520, lead screw 310 fixed connection is on support frame 4, be connected with the nut 330 of looks adaptation on the lead screw 310, the one end of lifting member 320 is connected with nut 330, lifting member 320 includes gyro wheel 320a, iron wire 320b and fixed block 320c, iron wire 320b is connected with gyro wheel 320a winding, gyro wheel 320a fixed connection is on support frame 4, the one end coupling nut 330 of iron wire 320b, the other end is connected with fixed block 320c, two sets of lifting member 320 mirror image settings.

The screw rod 310 is started to move left and right, the nut 330 drives the iron wire 320b, when the nut 330 moves to the left, the right iron wire 320b is pulled, the right fixed block 320c is lifted, the right fixed block 320c cannot touch the second switch 520, so that the second containing box 220 is in a closed state, the sodium hydroxide solution cannot be poured into the reaction box 110, when the nut 330 moves to the left, the left iron wire 320b naturally drops, the fixed block 320c touches the first switch 510, the first containing box 210 is opened, the tert-butyl hydroperoxide is poured into the reaction box 110, similarly, when the nut 330 moves to the right, the first containing box 210 is closed, the pouring of the tert-butyl hydroperoxide into the reaction box 110 is stopped, the second containing box 220 is opened, the sodium hydroxide solution is poured into the reaction box 110, and the device can avoid the sodium hydroxide solution and the tert-butyl hydroperoxide from being poured into the inner container 120 at the same time, the phenomenon that partial components cannot react due to accumulation caused by excessive pouring amount at the same time at one time is avoided, the amount of sodium salt is reduced, only one of the components is poured into the inner container 120 at the same time, and the condition that the component with less amount can be maximally reacted is ensured.

It should be noted that, by controlling the moving speed of the nut 330 and the touching time of the fixing block 320c, the amount of the sodium hydroxide solution or the t-butyl hydroperoxide poured into the inner container 120 can be determined, and there is no need to manually control the input amount, and there is no need to perform multiple operations due to the excessive amount of the sodium hydroxide solution and the t-butyl hydroperoxide.

The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.

The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the patent and protection scope of the present invention should be subject to the appended claims.

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