Production equipment and method of dibenzoyl peroxide

Abstract

Compared with the prior art, the dibenzoyl peroxide production equipment and method provided by the invention have the advantages that during peroxidation, the temperature is monitored in real time through a scanning calorimeter DSC (Differential Scanning Calorimeter); a hydrogen peroxide regulating valve, a circulating frozen saline water return regulating valve, a hydrogen peroxide dropwise adding switch valve, a discharging valve and a benzoyl chloride dropwise adding regulating valve are regulated in real time through a DCS (Distributed Control System) according to monitoring information, so that substances reacted in the peroxidation kettle can be synthesized under the optimal condition all the time, and the synthesis yield is increased; meanwhile, the stirrer accelerates mixing contact of reactants through stirring, and the reaction efficiency is improved.

Description

Technical Field

[0001] The invention relates to the technical field of dibenzoyl peroxide production, and in particular to a production device and a method for dibenzoyl peroxide. Background Art

[0002] Dibenzoyl peroxide is also known as benzoyl peroxide, commonly known as initiator BPO. At room temperature, dibenzoyl peroxide is a white crystalline powder with a slight bitter almond smell. It is soluble in benzene, chloroform, ether, and slightly soluble in ethanol and water. It can be used as a monomer polymerization initiator for polyvinyl chloride, unsaturated polyesters, polyacrylates, etc. It can also be used as a cross-linking agent for polyethylene and a rubber vulcanizer.

[0003] When the existing dibenzoyl peroxide equipment synthesizes dibenzoyl peroxide, the synthesis yield is only 96-97%, and the synthesis yield is low. Therefore, a production equipment and method for dibenzoyl peroxide are proposed. Summary of the invention

[0004] In order to solve at least one of the above technical shortcomings, the present invention provides a production equipment of dibenzoyl peroxide, including: SIS system, DCS automatic control system, scanning calorimeter DSC and sound and light alarm, the liquid alkali storage tank is connected to the liquid alkali high-level tank through a liquid alkali pump, a liquid level meter is arranged in the liquid alkali high-level tank, the liquid alkali high-level tank is connected to the peroxidation kettle, a stirrer is arranged in the peroxidation kettle, a coil is arranged inside the outer wall of the peroxidation kettle, the coil circulation chilled brine return water regulating valve is connected to the brine circulation tank, the refrigerator is connected to the brine circulation tank, the hydrogen peroxide raw material barrel is connected to the hydrogen peroxide high-level tank through a barrel pump and a feed valve, the bottom of the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide regulating valve, and the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide droplet The switch valve is connected to the peroxidation kettle, the benzoyl chloride material barrel is connected to the benzoyl chloride high-level tank through a vacuum pump and a benzoyl chloride feeding switch valve, the benzoyl chloride high-level tank is provided with a vent valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a discharge valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a benzoyl chloride dropping regulating valve, the peroxidation kettle is also connected to an emergency discharge valve and an emergency water injection valve, the SIS system and the DCS automatic control system are connected to the liquid level meter, the scanning calorimeter DSC, the hydrogen peroxide regulating valve, the hydrogen peroxide dropping switch valve, the sound and light alarm, the circulating chilled brine return water regulating valve, the vacuum pump, the discharge valve, the benzoyl chloride dropping regulating valve, the benzoyl chloride feeding switch valve, the emergency discharge valve and the emergency water injection valve by electrical signals.

[0005] Furthermore, it also includes a suction filtration cylinder, which is connected to the mother liquid tank through a mother liquid self-priming pump, and also includes an evaporator, a crystallizer, a packaging machine and a weighing sensor.

[0006] Furthermore, it also includes a material barrel, which is connected to a high-level tank through a diaphragm pump (P104), the high-level tank is connected to a foaming cylinder, the foaming cylinder is connected to a colloid mill disperser, the high-level tank is connected to the colloid mill disperser, the colloid mill disperser is connected to a detection machine, and the detection machine is connected to a kneading machine.

[0007] A production method of dibenzoyl peroxide is applied to a production device of dibenzoyl peroxide, and the method comprises: peroxidation, filtration, washing, drying, packaging, paste / paste production, salt-forming reaction, peroxidation reaction, solid-liquid separation, washing, pulping centrifugal mixing, centrifugal filtration, kneading and stirring, centrifugal separation and wastewater treatment.

[0008] Furthermore, peroxidation: the refrigerator is started before feeding, and the brine temperature in the brine circulation tank is cooled to -15°C in advance; the liquid alkali is pumped from the liquid alkali storage tank to the liquid alkali high-level tank through the liquid alkali pump, and is added to the peroxidation kettle at one time after liquid level measurement; the agitator of the peroxidation kettle is started, and the coiled chilled brine inlet and outlet circulating chilled brine return water regulating valve is opened; the feed valve is opened, and hydrogen peroxide is quantitatively pumped from the hydrogen peroxide raw material barrel to the hydrogen peroxide high-level tank with a barrel pump; when the temperature of the peroxidation kettle is between 5 and 15°C, the hydrogen peroxide regulating valve at the bottom of the hydrogen peroxide high-level tank is opened, and the hydrogen peroxide regulating valve and the circulating chilled brine return water regulating valve are adjusted by DCS temperature to automatically control the reaction temperature of the peroxidation kettle between 5 and 15°C. When the reaction temperature rises to 16°C, the sound and light alarm of the DCS automatic control system will send out a sound and light over-temperature alarm signal, the opening of the hydrogen peroxide dripping switch valve is "0%", and the opening of the circulating chilled brine return water regulating valve is "100%". At the same time, the DCS system interlocks to close the hydrogen peroxide dripping switch valve and stop dripping hydrogen peroxide to prevent the decomposition of hydrogen peroxide caused by excessive temperature; when the DCS system fails and the detected temperature reaches 35°C, the SIS system interlocks and closes the hydrogen peroxide regulating valve, opens the circulating chilled brine return water regulating valve urgently, and the emergency discharge valve and emergency water injection valve are used to urgently cool the temperature of the peroxidation kettle, and emergency water is injected and discharged in an accident; after the hydrogen peroxide is added, the liquid temperature is kept at 5~ 8℃, start the vacuum pump, close the vent valve of the benzoyl chloride high-level tank, open the feed valve, quantitatively extract benzoyl chloride from the benzoyl chloride barrel into the benzoyl chloride high-level tank through the vacuum pump, then close the vacuum valve and open the vent valve; open the discharge valve at the bottom of the benzoyl chloride high-level tank, adjust the opening of the benzoyl chloride dripping regulating valve through the DCS system temperature, slowly drip benzoyl chloride, and control the temperature of the peroxidation kettle between 5 and 15℃. When the temperature is high, adjust the benzoyl chloride dripping regulating valve to reduce the amount of material dripping, and at the same time open the circulating chilled brine return water regulating valve to increase the flow of circulating chilled brine, thereby reducing the temperature of the peroxidation kettle; when the reaction temperature rises to 16℃, the DCS automatic control system The sound and light alarm of the system will send out sound and light over-temperature alarm signals, the opening of the benzoyl chloride dripping regulating valve is "0%", the opening of the circulating chilled brine return water regulating valve is "100%", and at the same time, the DCS system interlocks to close the benzoyl chloride feed switch valve and stops dripping benzoyl chloride to prevent the hydrolysis of benzoyl chloride caused by excessive temperature; when the DCS system fails and the temperature further rises to 20°C, the SIS system sound and light alarm; when the detected temperature reaches 35°C, the emergency interlock closes the benzoyl chloride dripping regulating valve, and the chilled brine return water regulating valve, emergency discharge valve and emergency water injection valve are opened to urgently cool the temperature of the peroxidation kettle, and emergency water is injected and discharged; the reaction ends with the formation of crystalline benzoyl peroxide (di)

[0009] Further, filtering, washing, drying and packaging: putting benzoyl peroxide (di) crystals into a suction cylinder and filtering with a mother liquor self-priming pump, the filtrate is pumped into a mother liquor tank, and washed several times to remove sodium chloride and other impurities generated by the reaction. The washing wastewater is high-salt wastewater. After benzoic acid is crystallized and precipitated, it is evaporated and concentrated to produce sodium chloride salt. Benzoic acid and sodium chloride are both by-products. The washed crystals are then put into an automatic packaging machine and packaged into solid benzoyl peroxide (di) finished products; 1 / 4 of the solid finished product is used for compounding to produce paste / paste benzoyl peroxide (di)

[0010] Furthermore, paste / paste production: the solid finished product from the above process is added to the foaming material tank, and dibutyl phthalate is extracted from the material barrel by a diaphragm pump and added to the high-level tank. After being measured (the added amount is 30-40% of the product), it is added to the foaming material tank for dissolution and stirring, and then placed in a colloid mill disperser, and a certain amount of dibutyl phthalate is added and stirred at high speed. After the paste / paste product is inspected by an inspection machine and passed, it is placed in a kneading machine for filling, and the paste / paste packaged product is obtained.

[0011] Further, salt-forming reaction: at room temperature and pressure, 450 kg of synthetic mother liquid in the mother liquid tank is pumped into the peroxidation kettle through a centrifugal pump, and then 516 kg of fresh water is added through the water meter, the refrigerator is turned on for cooling, and the agitator of the peroxidation kettle is turned on for stirring, and then 740 kg of liquid alkali accurately measured from the liquid alkali high-level tank is added to the peroxidation kettle. When the temperature drops to 5-15 ° C, 322 kg of hydrogen peroxide pumped to the high-level tank by a centrifugal pump is slowly added dropwise, the dropping time is 10-30 min, the liquid material temperature is controlled at 5-15 ° C, and the temperature is kept warm for 5 min after the dropwise addition is completed, and the reaction is completed; peroxidation reaction: after the hydrogen peroxide is added dropwise, 750 kg of benzoyl chloride pumped to the high-level tank by a centrifugal pump is slowly added dropwise, and the dropwise addition is completed for 1 hour, and the reaction temperature is controlled at 5-15 ° C. After the dropwise addition is completed, the temperature is kept warm for 0.5 hours, and the reaction is completed after the granular BPO is generated; solid-liquid separation and washing: after the reaction is completed, the pump is transferred to the washing peroxidation In the kettle, there is a filter screen in the washing peroxidation kettle, through which solid-liquid separation is carried out to separate the synthetic mother liquor, and the synthetic mother liquor flows into the mother liquor tank for reuse, and the unused synthetic mother liquor goes to the acid adjustment tank, and the separation time is 0.25h; the remaining crude product in the washing peroxidation kettle; after solid-liquid separation, 1618.553kg of reused washing water is added through the water meter, and the crude product in the washing peroxidation kettle is stirred for 1h. After washing, solid-liquid separation is carried out, and the washing waste liquid is separated and sent to the acid adjustment tank, and the crude product continues to be washed in the washing peroxidation kettle; 1595kg of fresh water is added to the crude product in the washing peroxidation kettle through the water meter, and solid-liquid separation is carried out after washing. The washing separation is 0.5h, and the washing waste water is separated, and the washing waste water is reused once to washing 1, and the remaining washing waste water flows into the sewage treatment station in the factory for treatment; the washing is repeated 5 times (1595kg each time), and a total of 7975kg of fresh water is used, and the washing time is 2.5h.

[0012] Preferably, beating and centrifugal mixing: after the last washing of the solid-liquid separation and washing process, the water and material are self-flowing to the grinder for grinding, and 2550 kg of fresh water is added to the colloid mill disperser by water meter for grinding, and the water grinding and beating are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; after the centrifugation is completed, the BPO (623.317 kg) and 1720 kg of calcium carbonate after centrifugation are manually added into the mixer, and the finished product (di)benzoyl peroxide-2 is packaged after passing the inspection. 2 (BPO-22); Centrifugal filtration: Washing 2 process After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged. After passing the inspection, the finished product is obtained; the wastewater from the centrifugal filtration is sent to the sewage treatment station for treatment; Kneading and stirring: At room temperature and pressure, 670 kg of BPO-75 is manually poured into the kneader, and then 300 kg of DBP (dibutyl phthalate) which has been pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded by a screw to mix. The mixture is put into the mixer, and 30 kg of emulsifier is manually added into the mixer, and the mixer is started to stir for 0.5 h. After being fully stirred and mixed, it is squeezed into the packaging barrel to obtain the finished paste BPO; high-salt wastewater pretreatment (i.e., acidification reaction, the "mixture of synthetic mother liquor and first washing waste liquor" of the acidification reaction of the benzoyl peroxide (di)-50 (BPO-50) project and the benzoyl peroxide (di)-22 (BPO-22), benzoyl peroxide (di)-75 (BPO-75) and the paste BPO project is reacted after mixing, and the material ratio is the ratio after the materials of the two projects are mixed) : After the unused 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40°C, and 77.5kg 31% hydrochloric acid is pumped into the acid adjustment tank. The feeding time is 5-20min. After the feeding is completed, it is stirred for 2h and the pH is adjusted to 1-3; centrifugal separation: after the pH is adjusted, the material is discharged into the centrifuge and centrifuged for 2h to obtain by-product benzoic acid; wastewater treatment: the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

[0013] Preferably, beating and centrifugal mixing: after the last washing of the solid-liquid separation and washing process, the water and material are self-flowing to the grinder for grinding, and 2550 kg of fresh water is added to the colloid mill disperser by water meter for grinding, and the grinding and beating with water are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; after the centrifugation is completed, the BPO (623.317 kg) and 1252 kg of calcium carbonate after centrifugation are manually added to the mixer, and the finished product (di)benzoyl peroxide-27 is packaged after passing the inspection. (BPO-27); Centrifugal filtration: Washing 2 process After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged. After passing the inspection, the finished product is obtained; the wastewater from centrifugal filtration is sent to the sewage treatment station for treatment; Kneading and stirring: At normal temperature and pressure, 670kg BPO-75 is manually poured into the kneader, and then 300kg DBP (dibutyl phthalate) which has been pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded into the mixer through a screw. Then add 30kg of emulsifier into the mixer manually, start the mixer and stir for 0.5h, stir and mix thoroughly and squeeze into the packaging barrel to obtain the finished BPO paste; high-salt wastewater pretreatment (i.e., acidification reaction, the "mixture of synthetic mother liquor and first washing waste liquor" of the acidification reaction of the benzoyl peroxide (di)-50 (BPO-50) project and the benzoyl peroxide (di)-27 (BPO-27), benzoyl peroxide (di)-75 (BPO-75) and the paste BPO project is mixed and reacted, and the material ratio is the ratio of the two project materials mixed): recovery of unused After the 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40°C, and 77.5kg 31% hydrochloric acid is pumped into the acid adjustment tank. The feeding time is 5-20min. After the feeding is completed, it is stirred for 2h and the pH is adjusted to 1-3; centrifugal separation: after the pH is adjusted, the material is discharged into the centrifuge and centrifuged for 2h to obtain by-product benzoic acid; wastewater treatment (i.e. neutralization reaction): the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

[0014] Beneficial effects:

[0015] 1. Compared with the prior art, the present invention monitors the temperature in real time by means of a scanning calorimeter DSC during peroxidation, and adjusts the hydrogen peroxide regulating valve, the circulating chilled brine return regulating valve, the hydrogen peroxide dripping switch valve, the discharge valve and the benzoyl chloride dripping regulating valve in real time according to the monitoring information by means of a DCS system, so that the substances reacting inside the peroxidation kettle can always be synthesized under the best conditions, thereby improving the synthesis yield, and at the same time, the agitator accelerates the mixing contact of the reactants by stirring, thereby improving the reaction efficiency.

[0016] 2. Put the benzoyl peroxide (di) crystals into the filtration cylinder and use the mother liquor self-priming pump to filter. The filtrate is pumped into the mother liquor tank and washed several times to remove the sodium chloride and other impurities generated by the reaction. The washing wastewater is high-salt wastewater. After the benzoic acid is crystallized, it is evaporated and concentrated to produce sodium chloride salt. Benzoic acid and sodium chloride are sold as by-products. The washed crystals are then put into the automatic packaging machine to be packaged into solid benzoyl peroxide (di) finished products; 1 / 4 of the solid finished products are used for compounding and producing paste / paste benzoyl peroxide (di)

[0017] 3. Add the solid finished product from the above process into the foaming material tank, use a diaphragm pump to extract dibutyl phthalate DBP from the barrel and add it to the high-level tank. After metering (the amount added is 30-40% of the product), add it into the foaming material tank to dissolve and stir, then put it into a colloid mill disperser, add a certain amount of dibutyl phthalate and stir at high speed. After the paste / paste product is inspected and qualified, put it into the kneading machine for filling, and the paste / paste packaged product is obtained.

[0018] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings in conjunction with the embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the peroxidation equipment of the present invention.

[0020] Figure 2 It is a schematic diagram of the SIS system and DCS automatic control system of the present invention.

[0021] Figure 3 It is a schematic diagram of the solid-liquid separation of the present invention.

[0022] Figure 4 Schematic diagram of the paste / cream packaging of the present invention. DETAILED DESCRIPTION

[0023] Please refer to Figures 1 to 4 ;

[0024] The present embodiment provides a production device for dibenzoyl peroxide, including: an SIS system, a DCS automatic control system, a scanning calorimeter DSC and an audible and visual alarm, a liquid alkali storage tank is connected to a liquid alkali high-level tank through a liquid alkali pump, a liquid level gauge is arranged in the liquid alkali high-level tank, the liquid alkali high-level tank is connected to a peroxidation kettle, a stirrer is arranged in the peroxidation kettle, a coil is arranged inside the outer wall of the peroxidation kettle, a coil circulation chilled brine return water regulating valve is connected to the brine circulation tank, a refrigerator is connected to the brine circulation tank, a hydrogen peroxide raw material barrel is connected to a hydrogen peroxide high-level tank through a barrel pump and a feed valve, the bottom of the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide regulating valve, and the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide dripping switch valve. The benzoyl chloride material barrel is connected to the benzoyl chloride high-level tank through a vacuum pump and a benzoyl chloride feeding switch valve, the benzoyl chloride high-level tank is provided with a vent valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a discharge valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a benzoyl chloride dropping regulating valve, the peroxidation kettle is also connected with an emergency discharge valve and an emergency water injection valve, the SIS system and the DCS automatic control system are connected with the liquid level meter, the scanning calorimeter DSC, the hydrogen peroxide regulating valve, the hydrogen peroxide dropping switch valve, the sound and light alarm, the circulating chilled brine return water regulating valve, the vacuum pump, the discharge valve, the benzoyl chloride dropping regulating valve, the benzoyl chloride feeding switch valve, the emergency discharge valve and the emergency water injection valve by electrical signals.

[0025] In the specific implementation, the liquid alkali is pumped from the liquid alkali storage tank (V301A / B) to the liquid alkali high-level tank (V103A / B) through the liquid alkali pump (P301A / B), and is added to the peroxidation kettle (R101A~F) at one time after liquid level measurement.

[0026] Start the agitator of the peroxidation kettle and open the coil chilled brine inlet and outlet valves (the refrigerator (M502A / B) is started before feeding, and the brine temperature in the brine circulation tank V502 is cooled to -15°C in advance).

[0027] Open the feed valve and use a barrel pump (P101) to quantitatively pump hydrogen peroxide from the hydrogen peroxide raw material barrel into the hydrogen peroxide high-level tank (V101A~F).

[0028] When the temperature of the peroxidation kettle (R101A~F) is between 5 and 15°C, open the bottom discharge valve of the hydrogen peroxide high-level tank (V101A~F), and adjust the opening of the hydrogen peroxide regulating valve TV-101A~F and the circulating chilled brine return regulating valve TV-103A~F through DCS temperature to automatically control the reaction temperature of the peroxidation kettle between 5 and 15°C.

[0029] When the reaction temperature rises to 16°C, the DCS automatic control system will send out an audible and visual over-temperature alarm signal, the hydrogen peroxide dripping switch valve TV-101A~F will be opened to "0%", and the circulating chilled brine return water regulating valve TV-103A~F will be opened to "100%". At the same time, the DCS system interlocks and closes the hydrogen peroxide dripping switch valve KV-104A~F, stops dripping hydrogen peroxide, and prevents the decomposition of hydrogen peroxide caused by excessive temperature.

[0030] When the DCS system fails and the detected temperature reaches 35°C, the SIS system interlocks and shuts down TV-101A~F, and opens TV-103A~F, TXV-104A~F and TXV-105A~F urgently to cool down the reactor temperature, and then injects water and discharges the reactor in an emergency.

[0031] After the hydrogen peroxide is added, keep the liquid temperature between 5 and 8°C, open the vacuum pump P103A / B, close the vent valve of the benzoyl chloride high-level tank (V102A~F), open the feed valve, and quantitatively extract benzoyl chloride from the benzoyl chloride barrel into the benzoyl chloride high-level tank (V102A~F) through the vacuum pump P103A / B, then close the vacuum valve and open the vent valve. Open the discharge valve at the bottom of the benzoyl chloride high-level tank (V102A~F), adjust the opening of the benzoyl chloride drop regulating valve TV-102A~F through the DCS system temperature, slowly drop benzoyl chloride, and control the temperature of the reactor between 5 and 15°C. When the temperature is high, adjust the benzoyl chloride drop regulating valve TV-102A~F to reduce the amount of material added, and at the same time open the circulating chilled brine return regulating valve TV-103A~F to increase the flow of circulating chilled brine, thereby reducing the temperature of the peroxidation reactor. If the reaction temperature rises to 16°C, the DCS automatic control system will send out an audible and visual over-temperature alarm signal, the opening of the benzoyl chloride addition regulating valve TV-102A~F will be "0%", and the opening of the circulating chilled brine return regulating valve TV-103A~F will be "100%". At the same time, the DCS system interlocks and closes the benzoyl chloride feed switch valve KV-105A~F, stops the addition of benzoyl chloride, and prevents the hydrolysis of benzoyl chloride caused by excessive temperature.

[0032] When the DCS system fails and the temperature further rises to 20°C, the SIS system will sound and light alarms; when the detected temperature reaches 35°C, the emergency interlock shuts down TV-102A~F, and opens TV-103A~F, TXV-104A~F and TXV-105A~F urgently to cool down the reactor temperature, and urgently inject water and discharge the reactor in an accident.

[0033] The reaction ends with the formation of crystalline (di)benzoyl peroxide.

[0034] During peroxidation, the temperature is monitored in real time by a scanning calorimeter DSC, and the DCS system is used to adjust the hydrogen peroxide regulating valve, the circulating chilled brine return regulating valve (temperature control), the hydrogen peroxide dripping switch valve (fine-tuning the amount of hydrogen peroxide), the discharge valve and the benzoyl chloride dripping regulating valve (fine-tuning the amount of benzoyl chloride) in real time according to the monitoring information, so that the substances reacting inside the peroxidation kettle can always be synthesized under the best conditions, thereby improving the synthesis yield, and at the same time, the agitator is stirred to accelerate the mixing contact of the reactants and improve the reaction efficiency.

[0035] Liquid caustic soda pump (P301A / B) means there are two liquid caustic soda pumps, P301A and P301B;

[0036] Liquid alkali storage tank (V301A / B) means there are two liquid alkali storage tanks, V301A and V301B;

[0037] Liquid caustic soda high-level tank (V103A / B) refers to two liquid caustic soda high-level tanks, namely liquid caustic soda high-level tank V103A and liquid caustic soda high-level tank V103B;

[0038] The peroxidation kettles (R101A to F) are: peroxidation kettle R101A, peroxidation kettle R101B, peroxidation kettle R101C, peroxidation kettle R101D, peroxidation kettle R101E and peroxidation kettle R101AF;

[0039] The refrigerators (M502A / B) are: refrigerator M502A and refrigerator M502B;

[0040] The hydrogen peroxide high-level tanks (V101A-F) are: hydrogen peroxide high-level tank V101A, hydrogen peroxide high-level tank V101B, hydrogen peroxide high-level tank V101C, hydrogen peroxide high-level tank V101D, hydrogen peroxide high-level tank V101E and hydrogen peroxide high-level tank V101F;

[0041] The hydrogen peroxide regulating valves (TV-101A~F) are: hydrogen peroxide regulating valve TV-101A, hydrogen peroxide regulating valve TV-101B, hydrogen peroxide regulating valve TV-101C, hydrogen peroxide regulating valve TV-101D, hydrogen peroxide regulating valve TV-101E and hydrogen peroxide regulating valve TV-101F;

[0042] The circulating chilled brine return water regulating valves (TV-103A~F) are respectively: circulating chilled brine return water regulating valve TV-103A, circulating chilled brine return water regulating valve TV-103B, circulating chilled brine return water regulating valve TV-103C, circulating chilled brine return water regulating valve TV-103D, circulating chilled brine return water regulating valve TV-103E and circulating chilled brine return water regulating valve TV-103F;

[0043] The hydrogen peroxide dripping switch valves (KV-104A~F) are respectively: hydrogen peroxide dripping switch valve KV-104A, hydrogen peroxide dripping switch valve KV-104B, hydrogen peroxide dripping switch valve KV-104C, hydrogen peroxide dripping switch valve KV-104D, hydrogen peroxide dripping switch valve KV-104E, hydrogen peroxide dripping switch valve KV-104F;

[0044] The emergency discharge valves (TXV-104A~F) are respectively: emergency discharge valve TXV-104A, emergency discharge valve TXV-104B, emergency discharge valve TXV-104C, emergency discharge valve TXV-104D, emergency discharge valve TXV-104E and emergency discharge valve TXV-104F.

[0045] The emergency water injection valves (TXV-105A~F) are: emergency water injection valve TXV-105A, emergency water injection valve TXV-105B, emergency water injection valve TXV-105C, emergency water injection valve TXV-105D, emergency water injection valve TXV-105E and emergency water injection valve TXV-105F.

[0046] The benzoyl chloride high-level tanks (V102A~F) are respectively: benzoyl chloride high-level tank V102A, benzoyl chloride high-level tank V102B, benzoyl chloride high-level tank V102C, benzoyl chloride high-level tank V102D, benzoyl chloride high-level tank V102E and benzoyl chloride high-level tank V102F.

[0047] The bottom discharge valves of the benzoyl chloride high-level tank (V102A~F) are also provided with A~F, which are discharge valve A, discharge valve B, discharge valve C, discharge valve D, discharge valve E and discharge valve F respectively.

[0048] The benzoyl chloride dropping regulating valves (TV-102A~F) are respectively: benzoyl chloride dropping regulating valve TV-102A, benzoyl chloride dropping regulating valve TV-102B, benzoyl chloride dropping regulating valve TV-102C, benzoyl chloride dropping regulating valve TV-102D, benzoyl chloride dropping regulating valve TV-102E and benzoyl chloride dropping regulating valve TV-102F.

[0049] The others A to F are all equipped with A, B, C, D, E, and F.

[0050] Other A / B are configured with A and B.

[0051] Furthermore, it also includes a suction filtration cylinder, which is connected to the mother liquid tank through a mother liquid self-priming pump, and also includes an evaporator, a crystallizer, a packaging machine and a weighing sensor.

[0052] In the specific implementation, the benzoyl peroxide (di) crystals are placed in a suction filtration cylinder (X101A-L) and filtered with a mother liquor self-priming pump P102, and the filtrate is pumped into a mother liquor tank (V104A / B), and washed multiple times to remove the sodium chloride and other impurities generated by the reaction. The washing wastewater is high-salt wastewater, and benzoic acid is crystallized and precipitated, and then evaporated and concentrated to produce sodium chloride salt. Benzoic acid and sodium chloride are sold as by-products. The washed crystals are then put into an automatic packaging machine to be packaged into solid benzoyl peroxide (di) finished products; 1 / 4 of the solid finished products are used for compounding and producing paste / paste benzoyl peroxide (di) salt.

[0053] Furthermore, it also includes a material barrel, which is connected to a high-level tank through a diaphragm pump (P104), the high-level tank is connected to a foaming cylinder, the foaming cylinder is connected to a colloid mill disperser, the high-level tank is connected to the colloid mill disperser, the colloid mill disperser is connected to a detection machine, and the detection machine is connected to a kneading machine.

[0054] In the specific implementation, the solid finished product from the above process is added to the foaming material cylinder M101A~D, E, and dibutyl phthalate DBP is extracted from the barrel by a diaphragm pump (P104) and added to the high-level tank (V106A / B). After being measured (the added amount is 30-40% of the product), it is added to the foaming material cylinder for dissolution and stirring, and then placed in the colloid mill disperser M102, and a certain amount of dibutyl phthalate is added and stirred at high speed. After the paste / paste product is inspected and qualified, it is placed in the kneading machine X103 for filling, and the paste / paste packaged product is obtained.

[0055] The colloid mill disperser is equipped with a grinding mechanism, a centrifugal mechanism and a filtering mechanism.

[0056] Further, washing, drying, packaging, paste / paste production, salt formation reaction, peroxidation reaction, solid-liquid separation, washing, pulping centrifugal mixing, centrifugal filtration, kneading and stirring, centrifugal separation and wastewater treatment.

[0057] Furthermore, peroxidation: the refrigerator is started before feeding, and the brine temperature in the brine circulation tank is cooled to -15°C in advance; the liquid alkali is pumped from the liquid alkali storage tank to the liquid alkali high-level tank through the liquid alkali pump, and is added to the peroxidation kettle at one time after liquid level measurement; the agitator of the peroxidation kettle is started, and the coiled chilled brine inlet and outlet circulating chilled brine return water regulating valve is opened; the feed valve is opened, and hydrogen peroxide is quantitatively pumped from the hydrogen peroxide raw material barrel to the hydrogen peroxide high-level tank with a barrel pump; when the temperature of the peroxidation kettle is between 5 and 15°C, the hydrogen peroxide regulating valve at the bottom of the hydrogen peroxide high-level tank is opened, and the hydrogen peroxide regulating valve and the circulating chilled brine return water regulating valve are adjusted by DCS temperature to automatically control the reaction temperature of the peroxidation kettle between 5 and 15°C. When the reaction temperature rises to 16°C, the sound and light alarm of the DCS automatic control system will send out a sound and light over-temperature alarm signal, the opening of the hydrogen peroxide dripping switch valve is "0%", and the opening of the circulating chilled brine return water regulating valve is "100%". At the same time, the DCS system interlocks to close the hydrogen peroxide dripping switch valve and stop dripping hydrogen peroxide to prevent the decomposition of hydrogen peroxide caused by excessive temperature; when the DCS system fails and the detected temperature reaches 35°C, the SIS system interlocks and closes the hydrogen peroxide regulating valve, opens the circulating chilled brine return water regulating valve urgently, and the emergency discharge valve and emergency water injection valve are used to urgently cool the temperature of the peroxidation kettle, and emergency water is injected and discharged in an accident; after the hydrogen peroxide is added, the liquid temperature is kept at 5~ 8℃, start the vacuum pump, close the vent valve of the benzoyl chloride high-level tank, open the feed valve, quantitatively extract benzoyl chloride from the benzoyl chloride barrel into the benzoyl chloride high-level tank through the vacuum pump, then close the vacuum valve and open the vent valve; open the discharge valve at the bottom of the benzoyl chloride high-level tank, adjust the opening of the benzoyl chloride dripping regulating valve through the DCS system temperature, slowly drip benzoyl chloride, and control the temperature of the peroxidation kettle between 5 and 15℃. When the temperature is high, adjust the benzoyl chloride dripping regulating valve to reduce the amount of material dripping, and at the same time open the circulating chilled brine return water regulating valve to increase the flow of circulating chilled brine, thereby reducing the temperature of the peroxidation kettle; when the reaction temperature rises to 16℃, the DCS automatic control system The sound and light alarm of the system will send out sound and light over-temperature alarm signals, the opening of the benzoyl chloride dripping regulating valve is "0%", the opening of the circulating chilled brine return water regulating valve is "100%", and at the same time, the DCS system interlocks to close the benzoyl chloride feed switch valve and stops dripping benzoyl chloride to prevent the hydrolysis of benzoyl chloride caused by excessive temperature; when the DCS system fails and the temperature further rises to 20°C, the SIS system sound and light alarm; when the detected temperature reaches 35°C, the emergency interlock closes the benzoyl chloride dripping regulating valve, and the chilled brine return water regulating valve, emergency discharge valve and emergency water injection valve are opened to urgently cool the temperature of the peroxidation kettle, and emergency water is injected and discharged; the reaction ends with the formation of crystalline benzoyl peroxide (di)

[0058] Further, filtering, washing, drying and packaging: putting benzoyl peroxide (di) crystals into a suction cylinder and filtering with a mother liquor self-priming pump, the filtrate is pumped into a mother liquor tank, and washed several times to remove sodium chloride and other impurities generated by the reaction. The washing wastewater is high-salt wastewater. After benzoic acid is crystallized and precipitated, it is evaporated and concentrated to produce sodium chloride salt. Benzoic acid and sodium chloride are both by-products. The washed crystals are then put into an automatic packaging machine and packaged into solid benzoyl peroxide (di) finished products; 1 / 4 of the solid finished product is used for compounding to produce paste / paste benzoyl peroxide (di)

[0059] Furthermore, paste / paste production: the solid finished product from the above process is added to the foaming material tank, and dibutyl phthalate is extracted from the material barrel by a diaphragm pump and added to the high-level tank. After being measured (the added amount is 30-40% of the product), it is added to the foaming material tank for dissolution and stirring, and then placed in a colloid mill disperser, and a certain amount of dibutyl phthalate is added and stirred at high speed. After the paste / paste product is inspected by an inspection machine and passed, it is placed in a kneading machine for filling, and the paste / paste packaged product is obtained.

[0060] Further, salt-forming reaction: at room temperature and pressure, 450 kg of synthetic mother liquid in the mother liquid tank is pumped into the peroxidation kettle through a centrifugal pump, and then 516 kg of fresh water is added through the water meter, the refrigerator is turned on for cooling, and the agitator of the peroxidation kettle is turned on for stirring, and then 740 kg of liquid alkali accurately measured from the liquid alkali high-level tank is added to the peroxidation kettle. When the temperature drops to 5-15 ° C, 322 kg of hydrogen peroxide pumped to the high-level tank by a centrifugal pump is slowly added dropwise, the dropping time is 10-30 min, the liquid material temperature is controlled at 5-15 ° C, and the temperature is kept warm for 5 min after the dropwise addition is completed, and the reaction is completed; peroxidation reaction: after the hydrogen peroxide is added dropwise, 750 kg of benzoyl chloride pumped to the high-level tank by a centrifugal pump is slowly added dropwise, and the dropwise addition is completed for 1 hour, and the reaction temperature is controlled at 5-15 ° C. After the dropwise addition is completed, the temperature is kept warm for 0.5 hours, and the reaction is completed after the granular BPO is generated; solid-liquid separation and washing: after the reaction is completed, the pump is transferred to the washing peroxidation In the kettle, there is a filter screen in the washing peroxidation kettle, through which solid-liquid separation is carried out to separate the synthetic mother liquor, and the synthetic mother liquor flows into the mother liquor tank for reuse, and the unused synthetic mother liquor goes to the acid adjustment tank, and the separation time is 0.25h; the remaining crude product in the washing peroxidation kettle; after solid-liquid separation, 1618.553kg of reused washing water is added through the water meter, and the crude product in the washing peroxidation kettle is stirred for 1h. After washing, solid-liquid separation is carried out, and the washing waste liquid is separated and sent to the acid adjustment tank, and the crude product continues to be washed in the washing peroxidation kettle; 1595kg of fresh water is added to the crude product in the washing peroxidation kettle through the water meter, and solid-liquid separation is carried out after washing. The washing separation is 0.5h, and the washing waste water is separated, and the washing waste water is reused once to washing 1, and the remaining washing waste water flows into the sewage treatment station in the factory for treatment; the washing is repeated 5 times (1595kg each time), and a total of 7975kg of fresh water is used, and the washing time is 2.5h.

[0061] Preferably, beating and centrifugal mixing: after the last washing of the solid-liquid separation and washing process, the water and material are self-flowing to the grinder for grinding, and 2550 kg of fresh water is added to the colloid mill disperser by water meter for grinding, and the water grinding and beating are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; after the centrifugation is completed, the BPO (623.317 kg) and 1720 kg of calcium carbonate after centrifugation are manually added into the mixer, and the finished product (di)benzoyl peroxide-2 is packaged after passing the inspection. 2 (BPO-22); Centrifugal filtration: Washing 2 process After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged. After passing the inspection, the finished product is obtained; the wastewater from the centrifugal filtration is sent to the sewage treatment station for treatment; Kneading and stirring: At normal temperature and pressure, 670 kg of BPO-75 is manually poured into the kneader, and then 300 kg of DBP (dibutyl phthalate) which has been pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded by a screw to mix. The mixture is put into the mixer, and 30 kg of emulsifier is manually added into the mixer, and the mixer is started to stir for 0.5 h. After being fully stirred and mixed, it is squeezed into the packaging barrel to obtain the finished paste BPO; high-salt wastewater pretreatment (i.e., acidification reaction, the "mixture of synthetic mother liquor and first washing waste liquor" of the acidification reaction of the benzoyl peroxide (di)-50 (BPO-50) project and the benzoyl peroxide (di)-22 (BPO-22), benzoyl peroxide (di)-75 (BPO-75) and the paste BPO project is reacted after mixing, and the material ratio is the ratio after the materials of the two projects are mixed) : After the unused 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40°C, and 77.5kg 31% hydrochloric acid is pumped into the acid adjustment tank. The feeding time is 5-20min. After the feeding is completed, it is stirred for 2h and the pH is adjusted to 1-3; centrifugal separation: after the pH is adjusted, the material is discharged into the centrifuge and centrifuged for 2h to obtain by-product benzoic acid; wastewater treatment: the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

[0062] Preferably, beating and centrifugal mixing: after the last washing of the solid-liquid separation and washing process, the water and material are self-flowing to the grinder for grinding, and 2550 kg of fresh water is added to the colloid mill disperser by water meter for grinding, and the grinding and beating with water are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; after the centrifugation is completed, the BPO (623.317 kg) and 1252 kg of calcium carbonate after centrifugation are manually added to the mixer, and the finished product (di)benzoyl peroxide-27 is packaged after passing the inspection. (BPO-27); Centrifugal filtration: Washing 2 process After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged. After passing the inspection, the finished product is obtained; the wastewater from centrifugal filtration is sent to the sewage treatment station for treatment; Kneading and stirring: At normal temperature and pressure, 670kg BPO-75 is manually poured into the kneader, and then 300kg DBP (dibutyl phthalate) which has been pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded into the mixer through a screw. Then add 30kg of emulsifier into the mixer manually, start the mixer and stir for 0.5h, stir and mix thoroughly and squeeze into the packaging barrel to obtain the finished BPO paste; high-salt wastewater pretreatment (i.e., acidification reaction, the "mixture of synthetic mother liquor and first washing waste liquor" of the acidification reaction of the benzoyl peroxide (di)-50 (BPO-50) project and the benzoyl peroxide (di)-27 (BPO-27), benzoyl peroxide (di)-75 (BPO-75) and the paste BPO project is mixed and reacted, and the material ratio is the ratio of the two project materials mixed): recovery of unused After the 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40°C, and 77.5kg 31% hydrochloric acid is pumped into the acid adjustment tank. The feeding time is 5-20min. After the feeding is completed, it is stirred for 2h and the pH is adjusted to 1-3; centrifugal separation: after the pH is adjusted, the material is discharged into the centrifuge and centrifuged for 2h to obtain by-product benzoic acid; wastewater treatment (i.e. neutralization reaction): the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

Claims

1. A production equipment for dibenzoyl peroxide, comprising: SIS system, DCS automatic control system, scanning calorimeter DSC and sound and light alarm built in the DCS automatic control system, characterized in that: the liquid alkali storage tank is connected to the liquid alkali high-level tank through a liquid alkali pump, a liquid level gauge is arranged in the liquid alkali high-level tank, the liquid alkali high-level tank is connected to the peroxidation kettle, a stirrer is arranged in the peroxidation kettle, a coil is arranged inside the outer wall of the peroxidation kettle, a coil circulation chilled brine return water regulating valve is connected to the brine circulation tank, a refrigerator is connected to the brine circulation tank, a hydrogen peroxide raw material barrel is connected to the hydrogen peroxide high-level tank through a barrel pump and a feed valve, the bottom of the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide regulating valve, and the hydrogen peroxide high-level tank is connected to the peroxidation kettle through a hydrogen peroxide dripping switch valve. The benzoyl chloride material barrel is connected to the benzoyl chloride high-level tank through a vacuum pump and a benzoyl chloride feed switch valve, the benzoyl chloride high-level tank is provided with a vent valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a discharge valve, the benzoyl chloride high-level tank is connected to the peroxidation kettle through a benzoyl chloride drop-adding regulating valve, the peroxidation kettle is also connected with an emergency discharge valve and an emergency water injection valve, the SIS system and the DCS automatic control system are connected with the liquid level meter, the scanning calorimeter DSC, the hydrogen peroxide regulating valve, the hydrogen peroxide drop-adding switch valve, the sound and light alarm, the circulating chilled brine return water regulating valve, the vacuum pump, the discharge valve, the benzoyl chloride drop-adding regulating valve, the benzoyl chloride feed switch valve, the emergency discharge valve and the emergency water injection valve by electrical signals.

2. A production equipment for dibenzoyl peroxide according to claim 1, characterized in that: It also includes a suction filter cylinder, which is connected to the mother liquid tank through a mother liquid self-priming pump, and also includes an evaporator, a crystallizer, a packaging machine and a weighing sensor.

3. A production equipment for dibenzoyl peroxide according to claim 2, characterized in that: It also includes a material barrel, which is connected to a high-level tank through a diaphragm pump (P104), the high-level tank is connected to a foaming cylinder, the foaming cylinder is connected to a colloid mill disperser, the high-level tank is connected to the colloid mill disperser, the colloid mill disperser is connected to a detection machine, and the detection machine is connected to a kneading machine.

4. A method for producing dibenzoyl peroxide, characterized in that: The production equipment of dibenzoyl peroxide used in claim 3 comprises the following methods: peroxidation, filtration, washing, drying, packaging, paste / paste production, salt-forming reaction, peroxidation reaction, solid-liquid separation, washing, pulping centrifugal mixing, centrifugal filtration, kneading and stirring, centrifugal separation and wastewater treatment.

5. A method for producing dibenzoyl peroxide according to claim 4, characterized in that: Peroxidation: Start the refrigerator before feeding, and cool the brine in the brine circulation tank to -15℃ in advance; pump the liquid alkali from the liquid alkali storage tank to the liquid alkali high-level tank through the liquid alkali pump, and add it to the peroxidation kettle at one time after liquid level measurement; start the agitator of the peroxidation kettle, open the coil chilled brine in and out circulating chilled brine return water regulating valve; open the feed valve, and pump hydrogen peroxide from the hydrogen peroxide raw material barrel to the hydrogen peroxide high-level tank with a barrel pump; when the temperature of the peroxidation kettle is between 5 and 15℃, open the hydrogen peroxide regulating valve at the bottom of the hydrogen peroxide high-level tank, and automatically control the reaction temperature of the peroxidation kettle through the DCS temperature adjustment of the hydrogen peroxide regulating valve and the opening of the circulating chilled brine return water regulating valve. Between 5 and 15°C; when the reaction temperature rises to 16°C, the sound and light alarm of the DCS automatic control system will send out a sound and light over-temperature alarm signal, the opening of the hydrogen peroxide dripping switch valve is "0%", and the opening of the circulating chilled brine return water regulating valve is "100%". At the same time, the DCS system interlocks to close the hydrogen peroxide dripping switch valve and stop dripping hydrogen peroxide to prevent the decomposition of hydrogen peroxide caused by excessive temperature; when the DCS system fails and the detected temperature reaches 35°C, the SIS system interlocks and closes the hydrogen peroxide regulating valve, opens the circulating chilled brine return water regulating valve urgently, and the emergency discharge valve and emergency water injection valve are used to urgently cool the peroxidation kettle temperature, and emergency water injection and accident discharge are carried out; After the hydrogen peroxide is added, the temperature of the liquid is maintained between 5 and 8°C, the vacuum pump is turned on, the vent valve of the benzoyl chloride high-level tank is closed, the feed valve is opened, and the benzoyl chloride is quantitatively extracted from the benzoyl chloride barrel to the benzoyl chloride high-level tank through the vacuum pump, and then the vacuum valve is closed and the vent valve is opened; Open the discharge valve at the bottom of the benzoyl chloride high-level tank, adjust the opening of the benzoyl chloride dripping regulating valve through the DCS system temperature, slowly drip benzoyl chloride, and control the temperature of the peroxidation kettle between 5 and 15°C. When the temperature is high, adjust the benzoyl chloride dripping regulating valve to reduce the amount of material dripping, and at the same time open the circulating chilled brine return regulating valve to increase the flow of circulating chilled brine, thereby reducing the temperature of the peroxidation kettle; when the reaction temperature rises to 16°C, the sound and light alarm of the DCS automatic control system will send out an audible and visual over-temperature alarm signal, the opening of the benzoyl chloride dripping regulating valve is "0%, and the circulating chilled brine is turned on. The opening of the brine return water regulating valve is "100%". At the same time, the DCS system interlocks to close the benzoyl chloride feed switch valve and stops adding benzoyl chloride to prevent the hydrolysis of benzoyl chloride caused by excessive temperature. When the DCS system fails and the temperature further rises to 20°C, the SIS system sound and light alarms. When the detected temperature reaches 35°C, the emergency interlock closes the benzoyl chloride addition regulating valve, and the brine return water regulating valve, emergency discharge valve and emergency water injection valve are opened to urgently cool down the peroxidation kettle temperature, and emergency water is injected and discharged. The reaction ends with the formation of crystalline benzoyl peroxide (di) 6. A method for producing dibenzoyl peroxide according to claim 5, characterized in that: Filtration, washing, drying and packaging: put the benzoyl peroxide (di) crystals into a suction cylinder and filter with a mother liquor self-priming pump. The filtrate is pumped into a mother liquor tank and washed several times to remove the sodium chloride and other impurities generated by the reaction. The washing wastewater is high-salt wastewater. Benzoic acid is crystallized and then evaporated and concentrated to produce sodium chloride salt. Benzoic acid and sodium chloride are both by-products. The washed crystals are then put into an automatic packaging machine and packaged into solid benzoyl peroxide (di) finished products; 1 / 4 of the solid finished product is used for compounding to produce paste / paste benzoyl peroxide (di) 7. A method for producing dibenzoyl peroxide according to claim 6, characterized in that: Paste / paste production: the solid finished product from the above process is added to the foaming material tank, and dibutyl phthalate is extracted from the material barrel by a diaphragm pump and added to the high-level tank. After being measured (the added amount is 30-40% of the product), it is added to the foaming material tank for dissolution and stirring, and then placed in a colloid mill disperser, and a certain amount of dibutyl phthalate is added and stirred at high speed. After the paste / paste product is inspected by the inspection machine and passed, it is placed in the kneading machine for filling, and the paste / paste packaged product is obtained.

8. The method for producing dibenzoyl peroxide according to claim 7, characterized in that: salt-forming reaction: at normal temperature and pressure, 450 kg of synthetic mother liquid in the mother liquid tank is pumped into the peroxidation kettle via a centrifugal pump, and then 516 kg of fresh water is added via a water meter, the refrigerator is turned on for cooling, and the agitator of the peroxidation kettle is turned on for stirring, and then 740 kg of liquid alkali accurately measured from the liquid alkali header tank is added to the peroxidation kettle, and when the temperature is cooled to 5-15° C., 322 kg of hydrogen peroxide pumped to the header tank via a centrifugal pump in advance is slowly added dropwise, the dropping time is 10-30 min, the liquid material temperature is controlled at 5-15° C., and the temperature is kept warm for 5 min after the dropwise addition is completed, and the reaction is terminated; peroxidation reaction: after the hydrogen peroxide is added dropwise, 750 kg of benzoyl chloride pumped to the header tank via a centrifugal pump in advance is slowly added dropwise, and the dropwise addition is completed for 1 h, and the reaction temperature is controlled at 5-15° C. After the dropwise addition is completed, the temperature is kept warm for 0.5 h, and the reaction is terminated after the granular BPO is generated; solid-liquid separation and washing: reaction After completion, the product is transferred to the washing peroxidation kettle by a pump. There is a filter in the washing peroxidation kettle. The filter is used to separate the solid and liquid, separate the synthetic mother liquor, and the synthetic mother liquor flows into the mother liquor tank for reuse. The unused synthetic mother liquor goes to the acid adjustment tank, and the separation time is 0.25h; the remaining crude product in the washing peroxidation kettle; after solid-liquid separation, 1618.553kg of recycled washing water is added through the water meter, and the crude product in the washing peroxidation kettle is stirred for 1h. After washing, solid-liquid separation is performed, and the washing waste liquid is separated and sent to the acid adjustment tank, and the crude product continues to be washed in the washing peroxidation kettle; 1595kg of fresh water is added to the crude product in the washing peroxidation kettle through the water meter, and solid-liquid separation is performed after washing. The washing separation is 0.5h, and the washing waste water is separated. The washing waste water is reused once to washing 1, and the remaining washing waste water flows into the sewage treatment station in the factory for treatment; the washing is repeated 5 times (1595kg each time), and a total of 7975kg of fresh water is used, and the washing time is 2.5h.

9. A method for producing dibenzoyl peroxide according to claim 8, characterized in that: Beating and centrifugal mixing: After the last washing of the solid-liquid separation and washing process, the material flows to the grinder together with water and grinding. At the same time, 2550kg of fresh water is added to the colloid mill disperser by water meter for grinding. The grinding and beating with water are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; After centrifugation, BPO (623.317 kg) and 1720 kg of calcium carbonate are manually added to the mixer, and the finished product (di)benzoyl peroxide-22 (BPO-22) is packaged after passing the inspection; Centrifugal filtration: Washing 2 process: After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged, and the finished product is packaged after passing the inspection; The wastewater from centrifugal filtration is sent to the sewage treatment station for treatment; kneading and stirring: at normal temperature and pressure, 670kg BPO-75 is manually poured into the kneader, and then 300kg DBP (dibutyl phthalate) which is pre-pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded into the mixer through a screw, and then 30kg emulsifier is manually added to the mixer, and the mixer is started to stir for 0.5h. After fully stirring and mixing, it is squeezed into a packaging barrel to obtain a finished paste BPO; high-salt wastewater pretreatment (i.e., acidification reaction, (di) benzoyl peroxide-50 (BPO-50) project and (di) benzoyl peroxide-22 (BPO-22), (di) benzoyl peroxide-75 (BPO-75) ) and the "mixed liquid of synthetic mother liquor and first washing waste liquid" of the acidification reaction of the paste BPO project are mixed and reacted, and its material ratio is the ratio after the materials of the two projects are mixed): after the unused 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are recovered and pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40°C, and 77.5kg31% hydrochloric acid is pumped into the acid adjustment tank, the feeding time is 5-20min, and the feeding is completed. Stir for 2h and adjust the pH to 1-3; centrifugal separation: after the pH is adjusted, discharge the material into the centrifuge, and centrifuge for 2h to obtain by-product benzoic acid; wastewater treatment: the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

10. A method for producing dibenzoyl peroxide according to claim 7, characterized in that: Beating and centrifugal mixing: After the last washing of the solid-liquid separation and washing process, the material flows to the grinder together with water and grinding. At the same time, 2550kg of fresh water is added to the colloid mill disperser by water meter for grinding. The grinding and beating with water are carried out for 2 hours; the grinding material flows into the centrifugal mechanism in the colloid mill disperser for solid-liquid separation, and the centrifugal wastewater is sent to the factory sewage treatment station for treatment; After centrifugation, BPO (623.317 kg) and 1252 kg of calcium carbonate are manually added to the mixer, and the finished product (di)benzoyl peroxide-27 (BPO-27) is packaged after passing the inspection; Centrifugal filtration: Washing 2 process: After washing for 2 hours, the crystals are centrifuged and filtered at the filtering mechanism in the 3-in-1 colloid mill disperser, and the product BPO-75 is packaged, and the finished product is packaged after passing the inspection; The wastewater from centrifugal filtration is sent to the sewage treatment station for treatment; kneading and stirring: at normal temperature and pressure, 670kg BPO-75 is manually poured into the kneader, and then 300kg DBP (dibutyl phthalate) which is pre-pumped to the high-level tank by a diaphragm pump is added to the kneader. After BPO-75 and DBP are fully mixed, the kneader outlet is extruded into the mixer through a screw, and then 30kg emulsifier is manually added to the mixer, and the mixer is started to stir for 0.5h. After fully stirring and mixing, it is squeezed into a packaging barrel to obtain a finished paste BPO; high-salt wastewater pretreatment (i.e., acidification reaction, benzoyl peroxide (di)-50 (BPO-50) project and benzoyl peroxide (di)-27 (BPO-27), benzoyl peroxide (di)-75 (BPO-75) and paste The "mixed liquid of synthetic mother liquor and first washing waste liquid" of the acidification reaction of the BPO project is mixed and reacted, and its material ratio is the ratio of the materials of the two projects mixed): after the unused 1425.336kg synthetic mother liquor and 1743.101kg first washing waste liquid are recovered and pumped into the acid adjustment tank, the temperature in the kettle is controlled at 10-40℃, and 77.5kg31% hydrochloric acid is pumped into the acid adjustment tank. The feeding time is 5-20min. After the feeding is completed, it is stirred for 2h and the pH is adjusted to 1-3; centrifugal separation: after the pH is adjusted, the material is discharged into the centrifuge and centrifuged for 2h to obtain the by-product benzoic acid; wastewater treatment (i.e. neutralization reaction): the separated centrifugal 2 wastewater is combined with other wastewater and enters the brine neutralization tank to adjust the pH to neutral, and then enters the MVR evaporator in the factory for treatment.

Images