CN109701448A - A kind of apatite collecting agent dry solidification production method and equipment - Google Patents

A kind of apatite collecting agent dry solidification production method and equipment Download PDF

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Publication number
CN109701448A
CN109701448A CN201811391263.4A CN201811391263A CN109701448A CN 109701448 A CN109701448 A CN 109701448A CN 201811391263 A CN201811391263 A CN 201811391263A CN 109701448 A CN109701448 A CN 109701448A
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CN
China
Prior art keywords
collecting agent
vacuum chamber
dry solidification
apatite
reaction kettle
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Pending
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CN201811391263.4A
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Chinese (zh)
Inventor
刘浩然
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Institute Of Geology General Administration Of Geology And Mines Sinochem
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Institute Of Geology General Administration Of Geology And Mines Sinochem
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Priority to CN201811391263.4A priority Critical patent/CN109701448A/en
Publication of CN109701448A publication Critical patent/CN109701448A/en
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Abstract

The present invention proposes a kind of apatite collecting agent dry solidification production method and equipment, the method includes the steps: 1) saponification: reaction raw materials carry out saponification in reaction kettle, generate the collecting agent of lotion form;2) pressurization makes lotion form collecting agent enter heat exchange equipment, the moisture in collecting agent is set to heat up, then enter vacuum chamber interior walls by the hollow rotary shaft persistently rotated and sprayed from nozzle, the water vapour in collecting agent is entrained by the flow of air using vacuum effectiveness and is condensed, to make moisture be discharged, the collecting agent after dehydration falls into the bottom of vacuum chamber;3) it is discharged by dual-screw pelletizer from the bottom discharging mouth of vacuum chamber, being granulated becomes graininess collecting agent.The drawbacks of apatite collecting agent dry solidification production method proposed by the present invention, the solid collecting agent of production can be transported with woven bags packaging, solved metal bucket transport and used.

Description

A kind of apatite collecting agent dry solidification production method and equipment
Technical field
The invention belongs to technical field of beneficiation, and in particular to a kind of production method and equipment of collecting agent.
Background technique
Phosphorus ore is important strategic resource, is mainly used in and prepares phosphate and phosphate fertilizer.The production pair of phosphate and phosphate fertilizer The requirement of rock phosphate in powder raw material has certain P2O5Content.The rock phosphate in powder phosphorus content that nature produces is limited, thus mostly in low product Position rock phosphate in powder needs to carry out ore dressing, to reach the requirement of high-quality rock phosphate in powder.Froth flotation is that current sulphur dioxide of phosphor chemical industry is applied A kind of most ore dressing modes.For such mineral, the more mode of industrial application is that phosphorus is selected in flotation.Apatite flotation collector Phosphorus technique is selected suitable for the flotation of such ore.
Collecting agent is that most important one kind beneficiation reagent, effect mainly keep mineral surfaces hydrophobic, drop in floating agent Low mineral surfaces wetability, to improve the floatability of mineral.Currently, common apatite collecting agent is oxidized paraffin wax soap, oil The fatty acids such as acid, the AW series collecting agent including our hospital's research and development.Apatite collecting agent production process be mainly esters and alkali into Capable saponification, saponification usually carry out in a kettle, are released after the reaction was completed using hose from reactor bottom. It is in lotion form, so can only be stored in metal bucket, barreled collecting agent wants transport since water content is higher in reaction product Ask that comparison is harsh and transportation cost is also higher, in addition ore dressing is also more troublesome when using barreled collecting agent.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to propose to a kind of productions of apatite collecting agent dry solidification Method.
Another object of the present invention is to propose a kind of apatite collecting agent dry solidification production equipment.
Realize the technical solution of the object of the invention are as follows:
A kind of apatite collecting agent dry solidification production method, comprising steps of
1) saponification: reaction raw materials carry out saponification in reaction kettle, generate the collecting agent of lotion form;
2) pressurization makes lotion form collecting agent enter heat exchange equipment, and the moisture in collecting agent is made to heat up, then by continuing The hollow rotary shaft of rotation enters vacuum chamber interior walls and sprays from nozzle, and the water vapour in collecting agent is made using vacuum effectiveness It is entrained by the flow of air and condenses, so that moisture be made to be discharged, the collecting agent after dehydration falls into the bottom of vacuum chamber;
3) it is discharged by dual-screw pelletizer from the bottom discharging mouth of vacuum chamber, being granulated becomes graininess collecting agent.
Wherein, in step 1), the raw material of reaction is the leftover bits and pieces and alkali (NaOH) of soybean oil refining, quality proportioning be (7~ 9):2;
Preferably, reaction kettle is heated using steam, after temperature of charge reaches 90 ± 5 DEG C, stops heating, at this time Start timing, after 2~3 hours, saponification is completed.
Wherein, for the heat exchange equipment using steam as heat medium, the pressure of the steam is 0.4~0.5Mpa,
The steam is also used to produce by boasting by the material heating in reaction kettle and material remaining in reaction kettle pipeline.
Wherein, the vacuum degree of the vacuum chamber is -0.08Mpa to -0.1Mpa.
A kind of apatite collecting agent dry solidification production equipment characterized by comprising answer kettle, gear pump, tubulation heat exchange Device, vacuum chamber, dual-screw pelletizer,
The gear pump is arranged in the discharge port of the reactor bottom, and the discharge port connects the pipe of the tubular heat exchanger The shell side of journey, the tubular heat exchanger is connected with jet chimney;
The outlet conduit of the tube side of the tubular heat exchanger connects the vacuum chamber, and the discharge gate of the vacuum chamber bottom is set It is equipped with dual-screw pelletizer.
Further, the reaction kettle is closed and pressed type reaction kettle, and heating tube is provided on reaction kettle inner wall, described to add Heat pipe is connected to the jet chimney;Preferably, filter screen is set on the discharge port of the reactor bottom.
Wherein, the outlet conduit of the tube side of the tubular heat exchanger is connected with rotary shaft, and the rotary shaft is protruded into from top In vacuum chamber, nozzle is provided in the rotary shaft, the position of nozzle is located at the top of vacuum chamber;Rotation axle portion more than nozzle It is divided into hollow.
Wherein, the aperture of the nozzle is slice shape, and length is horizontal direction, bore size be (14~16) mm × (1~ 3)mm。
Wherein, the vacuum chamber is connected with recoil tank and vacuum pump;Recoil tank is connected with vacuum chamber at top, vacuum pump Pump-line is connected with recoil tank, and recoil tank is connected with steam-water separator.The pump-line of vacuum pump is connected with recoil tank, avoids Fraction solids material is pumped into pipeline in pumping process, accordingly even when there are fraction solids to fall into recoil tank, periodically opens recoil The cleaning of pot bottom ring flange is all right.
Preferably, scraper is provided in the vacuum chamber, scraper is fixed on above the hollow rotary shaft, knife face close to Vacuum chamber interior walls, for the material sticked on inner wall to be scraped.
It is highly preferred that the dual-screw pelletizer outer layer is that have a sheaf space, the inside filling is the cold water flowed.
Advantage is the present invention compared with prior art:
In compared with the prior art, lotion collecting agent be can be only placed in metal bucket, to production, transport and mine using all Cause bigger trouble, apatite collecting agent dry solidification production method proposed by the present invention, the solid collecting agent of production The drawbacks of being transported with woven bags packaging, solving metal bucket transport and use.
Production equipment proposed by the present invention has the advantages that at low cost, process is simple, easy to operate, brings very to enterprise Good economic benefit.
Detailed description of the invention
Fig. 1 is the structure diagram of apatite collecting agent dry solidification production equipment of the present invention.
In figure,
1 is reaction kettle, and 2 be gear pump, and 3 be tubular heat exchanger, and 4 be jet chimney, and 5 be going out for the tube side of tubular heat exchanger Mouthful pipeline, 6 be vacuum chamber, and 7 be dual-screw pelletizer, and 8 be rotary shaft, and 9 be scraper, and 10 be nozzle, and 11 be steam-water separator, 12 It is recoil tank for vacuum pump, 13,14 be cooling pond, and 15 be buffer tank.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
In embodiment, unless otherwise specified, method therefor and equipment are the device and method of this field routine.
Test example
In order to produce graininess, collecting agent easy to package, we tested the nozzles of diversified forms.Material is sprayed from nozzle When be with certain pressure, the opening area of nozzle is suitable, if although the too small injection pressure of area will increase, It is that the amount of injection is smaller, with regard to small, the gear pump in front needs to adjust very slow treating capacity, is not so likely to result in pipeline blockage (material In pipeline the residence time it is too long may result in blockage, especially tubulation).If nozzle opening area is too big, eject The material come does not scatter sufficiently, and will affect drying effect, and moisture is not taken away sufficiently in material, what such material was fallen When vacuum chamber bottom, double helix pelletizer material cannot be twisted out (liquid cannot be discharged in double helix pelletizer, it need The solid at rear ceaselessly gives the solids pressure in front, constantly solid could be discharged, so the moisture of material cannot be too It is high).So if there is this problem using round nozzle.It used porous type instead later, each hole area was become smaller, discovery is also It is to be easy blocking.Strip spout is finally used, effect is relatively good, and the amount of injection and the drying effect after ejecting all compare reason Think.
By the test of various shapes, the nozzle effect of aperture elongated strip shaped is optimal, having a size of 15mm × 2mm, level side To.
Embodiment 1:
Referring to Fig. 1.A kind of apatite collecting agent dry solidification production equipment, comprising: reaction kettle 1, gear pump 2, tubulation change Hot device 3, vacuum chamber 6 (hothouse), dual-screw pelletizer 7 (auger), steam-water separator 11, recoil tank 13, vacuum pump 12.
The discharge port of 1 bottom of reaction kettle is provided with gear pump 2, and the discharge port is connected to the pipe of the tubular heat exchanger 3 The shell side of journey, the tubular heat exchanger 3 is connected with jet chimney 4;There are agitator arm, the discharge port of reactor bottom in reaction kettle Upper setting filter screen.
The outlet conduit 5 of the tube side of the tubular heat exchanger connects the vacuum chamber 6, the discharge gate of the vacuum chamber bottom It is provided with dual-screw pelletizer 7.Dual-screw pelletizer outer layer has a sheaf space, and the inside filling is the cold water flowed.
Wherein, the reaction kettle 1 is closed and pressed type reaction kettle, is provided with heating tube, the heating on reaction kettle inner wall Pipe is connected to the jet chimney.
The outlet conduit 5 of the tube side of the tubular heat exchanger 3 connects rotary shaft 8, and rotary shaft 8, which is located at, is connected to the vacuum The center of top of room 6, and protruding into vacuum chamber, is arranged nozzle 10 in rotary shaft, conveying material enter evacuated chamber's inner wall and from It is sprayed in nozzle 10.Nozzle bore is slice shape, and the position of size 15mm × 2mm, horizontal direction, nozzle are located at the upper of vacuum chamber Portion (from top at about 1/3 height);Rotary shaft be enter from vacuum chamber top dead center position (vacuum chamber top be cylinder Shape, lower part are cone), rotary shaft is driven by a motor, and motor is arranged in above vacuum chamber.Nozzle is not fixed to rotary shaft Bottom, but it is intermediate, that is to say, that rotary shaft bottom is solid there are also one section.It is rotated during material is sprayed from nozzle Axis ceaselessly rotates, to guarantee that material can equably be sprayed onto all directions.
The vacuum chamber is connected with recoil tank 13 and vacuum pump 12;Recoil tank is connected with vacuum chamber at top, vacuum pump 12 Pump-line with recoil tank be connected, avoid in pumping process by fraction solids material suction pipeline in, accordingly even when there is part Solid falls into recoil tank, and it is all right periodically to open recoil pot bottom ring flange cleaning.Recoil tank 13 is connected with steam-water separator 11. Cooling pond 14 is in outdoor, and buffer tank 15 is on steam-water separator, and also in outdoor, buffer tank 15 is exactly to make vacuum pumping The gas with vapor out enters wherein, so that steam is all become water, flows back to cooling pond 14 from the overflow port at top.
Scraper 9 is provided in vacuum chamber 6;Scraper is fixed on above the hollow rotary shaft, and knife face is close in vacuum chamber Wall scrapes the material sticked on inner wall.
The equipment for wherein needing electrical control to operate is gear pump, hothouse scraper, dual-screw pelletizer, vacuum pump, diving Pump.
The above equipment is original equipment except reaction kettle, about 180,000 yuan of other parts cost.5 operators when production Achievable production.Have the advantages that at low cost, process is simple, easy to operate, brings good economic benefit to enterprise.
Embodiment 2
A kind of apatite collecting agent dry solidification production method, using the equipment of embodiment 1 comprising step:
1) saponification: reaction raw materials carry out saponification in closed and pressed type reaction kettle, generate catching for lotion form Receive agent;
Wherein, the raw material of reaction is the leftover bits and pieces and alkali (NaOH) of soybean oil refining, quality proportioning 8:2.
It is heated using steam (reaction kettle inner wall has steam-heating pipe), after temperature of charge reaches 90 DEG C, Stop heating, start timing at this time, after 2 hours, saponification is completed.
2) pressurize the tube side for making lotion form collecting agent enter tubular heat exchanger, using steam as heat medium, the steam Pressure be 0.4-0.5Mpa, so that the moisture in collecting agent is heated up, evacuated chamber's inner wall then entered by hollow rotary shaft (60-70 DEG C of vacuum room temperature) is simultaneously sprayed from nozzle, and the vapor in collecting agent is made using the vacuumizing effect of air compressor machine It is entrained by the flow of air and enters condensing tower, so that moisture be made to be discharged, the collecting agent after dehydration falls into the bottom of vacuum chamber, catching after dehydration Receive the bottom that agent falls into vacuum chamber;
The vacuum degree of the vacuum chamber is -0.09Mpa.Vacuum pump will be opened in advance, when vacuum degree reaches -0.09MPa, Material can be made to enter vacuum chamber, worked always in dry materials process intermediate pump.
Material after tubulation heats, advance in the duct by continuation, when reaching vacuum chamber top, with vertical hollow rotation Axis is connected, and rotary shaft enters vacuum chamber by top center, and rotary shaft has the nozzle of a horizontal direction in internal vacuum chamber Material is sprayed.Scraper is fixed on above rotary shaft, and knife face scrapes the material sticked on inner wall close to vacuum chamber interior walls.
3) it is discharged by dual-screw pelletizer from bottom discharging mouth, the collecting agent water content after drying is greatly reduced, substantially Solid forms are had become, woven bags packaging can be used.
The steam is also used to blow out material remaining in pipeline to after the completion of the material heating and drying in reaction kettle Come, with anti-clogging.
Steam pressure reaches 0.4-0.5Mpa, and main there are three purposes, first is that the material heating in reaction kettle, second is that giving Tubulation heating, third is that material remaining in pipeline is produced by boasting after the completion of dry, with anti-clogging.
It is as follows that the present embodiment further provides for operating procedure:
1. observe boiler pressure arrival 0.4~0.5MPa pressure, drying system air-supplying valve is opened.
2. opening conveying pipeline, steam valve, confirmation pipeline, nozzle are unobstructed, close after No leakage.
3. opening immersible pump, the buffer tank 15 on cooling pond is filled into water and keeps balancing.
4. opening vacuum pump cooling water waits for that water outlet has clear water outflow, vacuum pump, pressure gauge above observation recoil tank are opened Pointer variation, until reaching -0.09MPa vacuum degree.
5. opening reactor bottom dispensing valve after confirmation reaction kettle drainage conduit is connect correctly with gear pump three-way valve.
6. after checking that gear pump revolution counter knob is in 0 position, gear pump motor switch is opened, after motor runs well, Revolution counter switch is opened, slow turning knob observation pointer reaches suitable rotational speed.The change of gear pump operational situation is kept a close eye on simultaneously Change until steady running.
7. opening hothouse scraper, dual-screw pelletizer is opened.Opening pelletizer cooling water makes water outlet have clear water outflow.
Manufactured collecting agent be it is granular, be probably diameter 5mm, length 20mm it is cylindric, but wherein or also There is certain moisture (about 15%~18%), collecting agent has bonding phenomenon there are also slightly viscous at this time after pack.After being further dried Moisture content can drop to 10%-15%, can directly pack.
It is discussed in detail although the contents of the present invention have passed through above-mentioned preferred embodiment, but it should be appreciated that above-mentioned retouches It states and is not considered as limitation of the present invention.It will be understood by those skilled in the art that being opened in this patent design and specific embodiment Under showing, some deformations that directly can be exported or associate from this patent disclosure and common sense, those of ordinary skill in the art It will recognize to can also be used between the substitution of other methods or the prior art and the equivalent change or modification of feature or feature Mutually different combination, can realize this patent description function and effect, no longer one by one for example, belong to this patent protection Range.

Claims (10)

1. a kind of apatite collecting agent dry solidification production method, which is characterized in that comprising steps of
1) saponification: reaction raw materials carry out saponification in reaction kettle, generate the collecting agent of lotion form;
2) pressurization makes lotion form collecting agent enter heat exchange equipment, and the moisture in collecting agent is made to heat up, then by persistently rotating Hollow rotary shaft enter vacuum chamber interior walls and sprayed from nozzle, make the water vapour in collecting agent by gas using vacuum effectiveness Stream is taken away and is condensed, so that moisture be made to be discharged, the collecting agent after dehydration falls into the bottom of vacuum chamber;
3) it is discharged by dual-screw pelletizer from the bottom discharging mouth of vacuum chamber, being granulated becomes graininess collecting agent.
2. apatite collecting agent dry solidification production method according to claim 1, which is characterized in that in step 1), instead The raw material answered is the leftover bits and pieces and alkali (NaOH) of soybean oil refining, and quality proportioning is (7~9): 2;
Preferably, reaction kettle is heated using steam, after temperature of charge reaches 90 ± 5 DEG C, stops heating, start at this time Timing, after 2~3 hours, saponification is completed.
3. apatite collecting agent dry solidification production method according to claim 1, which is characterized in that the heat exchange equipment Using steam as heat medium, the pressure of the steam is 0.4~0.5Mpa;
The steam is also used to produce by boasting by the material heating in reaction kettle and material remaining in reaction kettle pipeline.
4. apatite collecting agent dry solidification production method according to claim 1, which is characterized in that the vacuum chamber Vacuum degree is -0.08Mpa to -0.1Mpa.
5. a kind of apatite collecting agent dry solidification production equipment characterized by comprising reaction kettle, gear pump, tubulation heat exchange Device, vacuum chamber, dual-screw pelletizer,
The gear pump is arranged in the discharge port of the reactor bottom, and the discharge port connects the tube side of the tubular heat exchanger, The shell side of the tubular heat exchanger is connected with jet chimney;
The outlet conduit of the tube side of the tubular heat exchanger connects the vacuum chamber, and the discharge gate of the vacuum chamber bottom is provided with Dual-screw pelletizer.
6. apatite collecting agent dry solidification production equipment according to claim 5, which is characterized in that the reaction kettle is Closed and pressed type reaction kettle is provided with heating tube on reaction kettle inner wall, and the heating tube is connected to the jet chimney;It is preferred that Filter screen is arranged on the discharge port of the reactor bottom in ground.
7. apatite collecting agent dry solidification production equipment according to claim 5, which is characterized in that the tubulation heat exchange The outlet conduit of the tube side of device is connected with rotary shaft, and the rotary shaft protrudes into vacuum chamber from top, is arranged in the rotary shaft There is nozzle, the position of nozzle is located at the top of vacuum chamber;Rotation shaft portion more than nozzle is hollow.
8. apatite collecting agent dry solidification production equipment according to claim 7, which is characterized in that the nozzle is opened Hole is slice shape, and length is horizontal direction, and bore size is (14~16) mm × (1~3) mm.
9. apatite collecting agent dry solidification production equipment according to claim 5, which is characterized in that the vacuum chamber connects It is connected to recoil tank and vacuum pump;Recoil tank is connected with vacuum chamber at top, and the pump-line of vacuum pump is connected with recoil tank, recoils Tank is connected with steam-water separator.
10. according to the described in any item apatite collecting agent dry solidification production equipments of claim 5~9, which is characterized in that institute It states and is provided with scraper in vacuum chamber, scraper is fixed on above the hollow rotary shaft, and knife face is close to vacuum chamber interior walls;
Preferably, the dual-screw pelletizer outer layer is that have a sheaf space, and the inside filling is the cold water flowed.
CN201811391263.4A 2018-11-21 2018-11-21 A kind of apatite collecting agent dry solidification production method and equipment Pending CN109701448A (en)

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CN201811391263.4A CN109701448A (en) 2018-11-21 2018-11-21 A kind of apatite collecting agent dry solidification production method and equipment

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Application Number Priority Date Filing Date Title
CN201811391263.4A CN109701448A (en) 2018-11-21 2018-11-21 A kind of apatite collecting agent dry solidification production method and equipment

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6780831B2 (en) * 2001-02-02 2004-08-24 Raisio Benecol, Ltd. Process for separating unsaponifiable valuable substances from sulphate soap based materials
CN102600985A (en) * 2012-03-28 2012-07-25 四川晶大矿业科技有限公司 Mineral separation collector and using method thereof
CN206450032U (en) * 2017-01-23 2017-08-29 吉安天卓选矿药剂有限公司 A kind of vacuum drier for preparing collecting agent
CN206444576U (en) * 2017-01-23 2017-08-29 吉安天卓选矿药剂有限公司 A kind of energy-conserving and environment-protective vacuum plant for preparing collecting agent
CN107441747A (en) * 2017-09-27 2017-12-08 顾建东 A kind of vacuum spray dehydrator group and method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6780831B2 (en) * 2001-02-02 2004-08-24 Raisio Benecol, Ltd. Process for separating unsaponifiable valuable substances from sulphate soap based materials
CN102600985A (en) * 2012-03-28 2012-07-25 四川晶大矿业科技有限公司 Mineral separation collector and using method thereof
CN206450032U (en) * 2017-01-23 2017-08-29 吉安天卓选矿药剂有限公司 A kind of vacuum drier for preparing collecting agent
CN206444576U (en) * 2017-01-23 2017-08-29 吉安天卓选矿药剂有限公司 A kind of energy-conserving and environment-protective vacuum plant for preparing collecting agent
CN107441747A (en) * 2017-09-27 2017-12-08 顾建东 A kind of vacuum spray dehydrator group and method

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