CN208365983U - A kind of equipment that oxalic acid is dry - Google Patents

A kind of equipment that oxalic acid is dry Download PDF

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Publication number
CN208365983U
CN208365983U CN201820428238.8U CN201820428238U CN208365983U CN 208365983 U CN208365983 U CN 208365983U CN 201820428238 U CN201820428238 U CN 201820428238U CN 208365983 U CN208365983 U CN 208365983U
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oxalic acid
type dryer
rake type
voltage regulation
tank
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CN201820428238.8U
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廖恒安
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Wuzhou Whampoa Chemical Pharmaceutical Co Ltd
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Wuzhou Whampoa Chemical Pharmaceutical Co Ltd
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Abstract

The utility model discloses the equipment that a kind of oxalic acid is dry, including rake type dryer, vacuum voltage regulation tank, oxalic acid collecting tank, hydraulic ejector, pump and cooling water pipeline;The raking arm of raker stirrer is hollow structure with shaft and is connected to heating pipeline.It feeds intake;Material is stirred and heated by raker stirrer using heating pipeline;Circulation line is formed using pump, hydraulic ejector and oxalic acid collecting tank and negative pressure is generated to vacuum voltage regulation tank;It is passed through inert gas and takes away material moisture;Oxalic acid collecting tank is sent by hydraulic ejector after the pressure buffer that gas in rake type dryer is passed through vacuum voltage regulation tank;Material after will be dry in rake type dryer is discharged to obtain finished product anhydrous oxalic acid.The advantage is that the raker stirrer of hollow structure can make material heating quickly and stirring will not agglomerate.Using low temperature drying, temperature of charge keeps 80~90 DEG C for a long time, material can either be avoided to cause damages to oxalic acid drying and dewatering, and the case where can prevent oxalic acid from decomposing due to overheating.

Description

A kind of equipment that oxalic acid is dry
Technical field
The utility model relates to a kind of process equipments of oxalic acid.
Background technique
Anhydrous oxalic acid, i.e. ethanedioic acid are the strong acid in organic acid, colourless monocline sheet or prism crystallization or white powder End has stronger hygroscopicity, is soluble in ethyl alcohol, is dissolved in water, be slightly soluble in ether.Insoluble in benzene and chloroform, fusing point α type: 189.5 DEG C, β type: 182 DEG C.Oxalic acid starts to distil at 100 DEG C, and 125 DEG C of whens distil rapidly, and 157 DEG C of whens largely distil, and start to decompose. Oxalic acid to skin, mucous membrane is irritating and corrosiveness, oxalic acid can be used for producing the drugs such as antibiotic and borneol as raw material.
Anhydrous oxalic acid is the primary raw material for producing borneol, in the esterification reaction process of borneolum syntheticum, to the water of anhydrous oxalic acid It point requires high.The anhydrous oxalic acid quality bought in the market is extremely unstable, and by traffic condition, weather conditions influenced compared with Greatly.
Utility model content
In order to solve the quality problems of anhydrous oxalic acid, the utility model aim is to provide a kind of equipment that oxalic acid is dry. With high income, quality is stablized, free of contamination feature.
A kind of dry equipment of oxalic acid described in the utility model, comprising: for dry aqueous oxalic acid rake type dryer, For to rake type dryer provide pressure buffer vacuum voltage regulation tank, for collects gasification oxalic acid oxalic acid collecting tank, be used for pair Vacuum voltage regulation tank provides the hydraulic ejector, the pump for maintaining pipeline to recycle and the cooling water pipe for cooling down equipment of negative pressure Road;
The rake type dryer is equipped with for stirring and the raker stirrer of heated material, the raking arm and shaft of the raker stirrer For hollow structure and it is connected to heating pipeline;Rake type dryer is additionally provided with air inlet and exhaust outlet, and the exhaust outlet and vacuum are steady Press the connection of tank upper pipeline;The vacuum voltage regulation tank lower part is connect with pump conduit;The hydraulic ejector high-voltage end connection Oxalic acid collecting tank top, low-pressure end connect vacuum voltage regulation tank, water inlet end connection pump.
Preferably, condenser is additionally provided on the vacuum voltage regulation tank and rake type dryer connecting line.Condenser can be with The water vapour of vaporization is condensed into water again, and continues to cool down by vacuum voltage regulation tank, can not only reduce the power load of pump, but also can It reduces the temperature of hydraulic ejector and reduces the uptake of distillation oxalic acid, avoid distillation oxalic acid and be discharged into air.
Preferably, the oxalic acid collecting tank enters the setting gas of the entrance in oxalic acid collecting tank in hydraulic ejector high-voltage end Liquid/gas separator.On-condensible gas not soluble in water is separated from water by gas-liquid separator, in order to avoid be pumped into cavitation is caused and damage.
Preferably, it is additionally provided with recovery end, the recovery end is connect by pipeline with the mouth of a river is pumped out.It is generated in dehydration And the sour water being stored in oxalic acid collecting tank can transport recovery end and carry out sodium oxalate recycling, realize wastewater zero discharge.
Preferably, the heating pipeline is also connected with rake type dryer surface, for keeping the temperature to rake type dryer.
A kind of application method of oxalic acid drying equipment described in the utility model, comprising the following steps:
S1, it feeds intake to rake type dryer progress aqueous oxalic acid;
S2, material is stirred and heated by raker stirrer using heating pipeline;
S3, circulation line is formed using pump, hydraulic ejector and oxalic acid collecting tank and negative pressure is generated to vacuum voltage regulation tank;
S4, it is passed through inert gas and takes away material moisture;
S5, oxalic acid will be sent by hydraulic ejector after pressure buffer that the gas in rake type dryer passes through vacuum voltage regulation tank Collecting tank;
S6, it is discharged the material in rake type dryer after drying to obtain finished product anhydrous oxalic acid.
Preferably, gas-liquid separation is set on the circulation line of hydraulic ejector and oxalic acid collecting tank in the step S3 Device.
Preferably, the gas in the step S5 in rake type dryer enters back into vacuum voltage regulation after first passing through condenser Tank.
Preferably, further include step S7, the sour water in oxalic acid collecting tank is delivered to recovery end progress sodium oxalate recycling.
Preferably, 500~1000kg of aqueous oxalic acid is put into from the feeding port of rake type dryer first;After feeding intake, open Dynamic raker stirrer is stirred;Heating pipe valve is opened to heat material in rake type dryer;Heating and temperature control is 130 DEG C or more, heating time is 1~2 hour;Temperature of charge in rake type dryer is controlled at 85 DEG C or more;
After temperature of charge reaches 85 DEG C or more, opens pump and keep pressure in 0.2Mpa;Open the air inlet of rake type dryer Mouthful, nitrogen is slowly introducing in rake type dryer;Open the cooling water valve of condenser;Heating and temperature control is 130~145 DEG C, the temperature of charge of measurement in every 30 minutes;Whether observation rake type dryer material can dissolve, and reduce if there is dissolution phenomena Heating temperature is until insoluble;When temperature of charge >=90 DEG C, and when material does not melt, heating and temperature control is at 130 DEG C ~140 DEG C;
When temperature of charge is at 100 DEG C~105 DEG C, air inlet is closed, keeps this temperature 1~1.5 hour, then slowly heating Stop heating after to 120 DEG C;After 30 minutes, sampling Detection;During pattern detection, continue to keep negative pressure and stirring;Sample inspection After surveying result qualification, hydraulic ejector is closed;Carry out rake type dryer discharging;If pattern detection result is unqualified, after continuation of insurance It holds 100 DEG C~105 DEG C of temperature of charge to heat 1~2 hour, resampling detection is until qualified.
Preferably, the inert gas is nitrogen.
A kind of dry equipment of oxalic acid described in the utility model, the advantage is that, the raker stirrer of hollow structure can make Material heating is quickly and stirring will not agglomerate.Using low temperature drying, temperature of charge keeps 80~90 DEG C for a long time, can either be to grass Sour drying and dewatering, and the case where can prevent oxalic acid from decomposing due to overheating, avoid material from causing damages.It is passed through nitrogen, is quickly taken away The moisture of aqueous oxalic acid.Meanwhile being passed through nitrogen and be different from general drying equipment and pouring compressed air, it is dry that rake can be effectively reduced Oxygen concentration in dry device reduces dust and oxygen mix in rake type dryer to greatest extent, effectively prevents the safety of dust explosion Accident.It is collected in oxalic acid collecting tank in the sour water that dehydration generates, can transport recovery end and carry out sodium oxalate recycling, realize Wastewater zero discharge.Entire production process totally-enclosed, the dust for reducing production environment generate, and operating environment is conducive to employee.This The anhydrous oxalic acid of equipment production, quality are stablized, and oxalic acid content is 99.2% or more;High income, every batch of yield is 68.5% More than.Gas/liquid separator device is increased, the volume of oxalic acid collecting tank can be reduced, while can avoid the damage of pumping unit.
Detailed description of the invention
Fig. 1 is the dry device structure schematic diagram of oxalic acid described in the utility model.
Appended drawing reference: 100- rake type dryer, 101- feeding port, 102- discharge port, 103- air inlet, 104- exhaust outlet, 110- motor, 120- raker stirrer, 130- heat pipeline;200- vacuum voltage regulation tank, 210- condenser;300- oxalic acid collecting tank, 310- hydraulic ejector, 320- gas-liquid separator;400- water pump;500- cooling water pipeline;600- recovery end.
Specific embodiment
As shown in Figure 1, the equipment that a kind of oxalic acid described in the utility model is dry, mainly includes rake type dryer 100, adds Pipe line 130, vacuum voltage regulation tank 200, condenser 210, oxalic acid collecting tank 300, hydraulic ejector 310, pump 400, cooling water pipe Road 500 and recovery end 600.The pump 400 can be fluoroplastic pump.The cooling water pipeline 500 is according to each functional component Needs selectively carry out water-cooled cooling, stablized with controlling each part temperatures.
The rake type dryer 100 is pan structure, is equipped with hollow raker stirrer 120 in pot, 120 one end of raker stirrer with The transmission connection of motor 110, other end connection heating pipeline 130.The heating pipeline 130 can be heated by steam or liquid adds Heat, heating pipeline 130 also connect 100 surface of rake type dryer by coil pipe.100 top of rake type dryer be equipped with air inlet 103, Feeding port 101 and exhaust outlet 104, lower part are equipped with discharge port 102.Exhaust outlet 104 connects very after concatenating condenser 210 by pipeline Empty 200 top of vacuum tank.The low pressure of 200 lower part of vacuum voltage regulation tank and pump 400 piping connections, top also with hydraulic ejector 310 Piping connection is held, negative pressure is generated to vacuum voltage regulation tank 200 from hydraulic ejector 310 to 300 high-pressure injection of oxalic acid collecting tank.Institute Liquid is injected grass by the 400 composition circulation line of hydraulic ejector 310, oxalic acid collecting tank 300 and pump stated, hydraulic ejector 310 Gas-liquid separator 320 is first passed through before sour collecting tank 300 carries out gas-liquid separation.Pump 400 delivery outlet also with 600 pipeline of recovery end Connection carries out sodium oxalate recycling for the sour water in oxalic acid collecting tank 300 to be delivered to recovery end 600.
Wherein, rake type dryer 100 carries out automatically controlling stirring using PLC programming controller, can timing positive and negative rotation, stir Mix material.It is indirect heating agitated dryer, collet is set in pot body, steam passes through the hollow shaft of rotary joint and rotation It connects, hollow raking arm is set on axis and is connected to hollow shaft.It is such to design the usable floor area for not only having improved unit volume but also strong Diabatic process is changed, has improved heat transfer efficiency, to guarantee optimal heat-transfer effect.
Condenser 210 again can be condensed into the water vapour of vaporization water, and continue to cool down by vacuum voltage regulation tank 200, Not only the power load of pump 400 can be reduced, but also the temperature of hydraulic ejector 310 can be reduced and reduce the uptake of distillation oxalic acid.It keeps away Exempt from distillation oxalic acid to be discharged into air.
Oxalic acid collecting tank 300 not only plays the role of collecting a small amount of distillation oxalic acid, but also as hydraulic ejector 310 and pump 400 The water storing vessel of cycling use of water.It is cooling using the collet type of cooling to guarantee that its temperature is constant.The oxalic acid that a small amount of distillation comes out is in water It is sufficiently mixed in power injector 310 with water and is dissolved in water.On-condensible gas nitrogen not soluble in water etc. by gas-liquid separator 320 with Water separation, in order to avoid caused cavitation and damaged by the sucking of pump 400.
The effect of nitrogen: the nitrogen under normal temperature and pressure, relative humidity is related with temperature, i.e. its moisture content carried and temperature It is related.After the nitrogen under room temperature enters rake type dryer 100, temperature can be increased, while its portable moisture content also increases , this is equivalent to the relative humidity reduced in rake type dryer 100, is conducive to the dehydration of aqueous oxalic acid.
The working principle of oxalic acid drying equipment described in the utility model and oxalic acid drying equipment described in the utility model Application method is as follows.
500~1000kg of aqueous oxalic acid is put into from feeding port 101.
After feeding intake, the cover board of feeding port 101 and fastening are closed, agitating mode is changed to automatically.Open heating pipeline 130 Valve is heated, material in pot is heated.Vapor (steam) temperature control is heated at 130 DEG C or more, heating time is about 1~2 hour. Pay attention to observing the temperature of charge in pot, control at 85 DEG C or more.
After temperature of charge reaches 85 DEG C or more, pump 400, hydraulic ejector 310 are opened, keep pump pressure in 0.2Mpa; 103 valve of air inlet is opened, nitrogen is slowly introducing in pot, valve is half-open to be limited.
Open the cooling water valve of hydraulic ejector 310 on vacuum voltage regulation tank 200;Heat vapor (steam) temperature control 130~ 145 DEG C or so, an every 30 minutes temperature of charge of measurement simultaneously keep a record.Pay attention to observing whether oxalic acid can dissolve, as dissolved Phenomenon then reduces heating vapor (steam) temperature until insoluble.
When temperature of charge >=90 DEG C, and when material does not melt, heating vapor (steam) temperature control is between 130 DEG C~140 DEG C. Material slowly heats up, and when temperature of charge is at 100 DEG C~105 DEG C, closes 103 valve of air inlet, keeps this temperature 1~1.5 small When, then 120 DEG C are to slowly warm up to, stop heating.It after 30 minutes, shuts down, sampling chemical examination detection.
During sample test, continue to keep stirring in negative pressure and pot.After result of laboratory test is qualified, pump 400, water-jet are closed Device 310, rake type dryer 100 is transferred to rotates forward discharging manually.Discharge port 102 is closed after discharging, closes feeding port 101.
If result of laboratory test is unqualified, continue after keeping 100 DEG C~105 DEG C of temperature of charge heating 1~2 hour, then extract Sample detection, until detecting qualification.
The liquid level condition of vacuum voltage regulation tank 200 need to be kept a close eye on when operation, vacuum voltage regulation tank 200 need to be arranged within every 4 hours Water process.Pump the condensed water in vacuum voltage regulation tank 200;The sour water for being more than 1/3 or more in oxalic acid collecting tank 300 is pumped into recycling 600 distillation process are held to use.
It after discharging, weighs, records weight.Dried anhydrous oxalic acid need to be covered immediately and be transported in drying chamber as early as possible Storage, to prevent getting damp.
The characteristics of the utility model: using PLC programming controller, and control agitating mode rotates forward 10~30min, stops 5min, 10~30min is inverted, stops 5min, the endless form rotated forward again.Both forward and reverse directions alternate agitation avoids material from gathering, and is conducive to object Material is sufficiently heated.Using low temperature drying, temperature of charge keeps 80~90 DEG C for a long time, can either to aqueous oxalic acid drying and dewatering, The case where capable of preventing oxalic acid from decomposing due to overheating again, material is avoided to cause damages.
It is passed through nitrogen, quickly takes away the moisture of aqueous oxalic acid.Meanwhile nitrogen is poured, it is different from general drying equipment punching Enter compressed air, oxygen concentration in pot can be effectively reduced, reduces dust and oxygen mix in pot to greatest extent, effectively prevent to send out The safety accident of fecula dust explosion.
Dehydration is collected in oxalic acid collecting tank 300 in the sour water of generation, be can transport recovery end 600 and is carried out sodium oxalate Recycling, realizes wastewater zero discharge.Entire production process totally-enclosed, the dust for reducing production environment generate, and operating environment is advantageous In employee.The anhydrous oxalic acid of the method and equipment production, quality are stablized, and oxalic acid content is 99.2% or more;High income, every batch of Yield is 68.5% or more.Gas-liquid separator 320 is increased, the volume of oxalic acid collecting tank 300 can be reduced, while can avoid pump 400 damage.
For those skilled in the art, it can make other each according to the above description of the technical scheme and ideas The corresponding change of kind and deformation, and all these changes and deformation all should belong to the guarantor of the utility model claims Within the scope of shield.

Claims (5)

1. a kind of dry equipment of oxalic acid characterized by comprising for drying the rake type dryer (100) of aqueous oxalic acid, using In vacuum voltage regulation tank (200), the oxalic acid collecting tank for collecting gasification oxalic acid that rake type dryer (100) provided with pressure buffer (300), the hydraulic ejector (310) for vacuum voltage regulation tank (200) to be provided with negative pressure, the pump for maintaining pipeline to recycle (400) cooling water pipeline (500) and for cooling down equipment;
The rake type dryer (100) is equipped with for stirring and the raker stirrer of heated material (120), the raker stirrer (120) Raking arm and shaft be hollow structure and be connected to heating pipeline (130);Rake type dryer (100) be additionally provided with air inlet (103) and Exhaust outlet (104), the exhaust outlet (104) are connect with vacuum voltage regulation tank (200) upper pipeline;The vacuum voltage regulation tank (200) lower part and pump (400) piping connection;In hydraulic ejector (310) high-voltage end connection oxalic acid collecting tank (300) Portion, low-pressure end connect vacuum voltage regulation tank (200), water inlet end connection pump (400).
2. a kind of dry equipment of oxalic acid according to claim 1, which is characterized in that the vacuum voltage regulation tank (200) Condenser (210) are additionally provided with on rake type dryer (100) connecting line.
3. a kind of dry equipment of oxalic acid according to claim 1, which is characterized in that the oxalic acid collecting tank (300) Enter the setting of the entrance in oxalic acid collecting tank (300) gas-liquid separator (320) in hydraulic ejector (310) high-voltage end.
4. a kind of dry equipment of oxalic acid according to claim 1, which is characterized in that it is additionally provided with recovery end (600), it is described Recovery end (600) by pipeline with pump (400) water outlet connect.
5. a kind of dry equipment of oxalic acid according to claim 1, which is characterized in that the heating pipeline (130) is also Rake type dryer (100) surface is connected, for keeping the temperature to rake type dryer (100).
CN201820428238.8U 2018-03-28 2018-03-28 A kind of equipment that oxalic acid is dry Active CN208365983U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108286886A (en) * 2018-03-28 2018-07-17 梧州黄埔化工药业有限公司 A kind of method and apparatus of oxalic acid drying

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108286886A (en) * 2018-03-28 2018-07-17 梧州黄埔化工药业有限公司 A kind of method and apparatus of oxalic acid drying

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