阅读说明：本技术 一种从nf3生产中副产氟化氢铵及氟化钾的装置及工艺 (Device and process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production ) 是由 齐航 武建鹏 冀延治 宋富财 郑阳光 岳立平 张帅 杨少飞 于 2021-01-29 设计创作，主要内容包括：本发明公开了一种从NF3生产中副产氟化氢铵及氟化钾的装置及工艺,包括工作台,所述工作台的上端中部设有凹槽,所述凹槽内设有输送机构,所述工作台的上端两侧均固定有电动推杆,两个所述电动推杆的一端均固定有升降块,两个所述升降块的一端共同固定有升降板,所述升降板的上端一侧固定有安装架,本发明还提出了一种从NF3生产中副产氟化氢铵及氟化钾的工艺。本发明可通过瓶体的间歇性移动实现灌装及瓶盖的安装,有效的节省了人工成本,避免了粉尘飘出,提高了生产效率,本方法可将含镍含氟的危险废物消除,转化为副产品,减少了环境污染,且本方法可将原有需要花钱处理的危险废物转化为副产品,具有一定的经济效益。(The invention discloses a device and a process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production, which comprises a workbench, wherein a groove is arranged in the middle of the upper end of the workbench, a conveying mechanism is arranged in the groove, electric push rods are fixed on two sides of the upper end of the workbench, lifting blocks are fixed on one ends of the two electric push rods, a lifting plate is fixed on one end of each lifting block, a mounting frame is fixed on one side of the upper end of each lifting plate, and the invention further provides the process for producing the ammonium bifluoride and the potassium fluoride as the byproducts in NF3 production. The invention can realize filling and bottle cap installation by intermittent movement of the bottle body, effectively saves labor cost, avoids dust from flying out, improves production efficiency, can eliminate dangerous waste containing nickel and fluorine, converts the dangerous waste into byproducts, reduces environmental pollution, can convert the dangerous waste which needs expensive treatment into the byproducts, and has certain economic benefit.)

1. The utility model provides a device of by-product ammonium bifluoride and potassium fluoride in production from NF3, includes the workstation, its characterized in that: four corners of the lower end of the workbench are respectively fixed with a bearing rod, the middle part of the upper end of the workbench is provided with a groove, and a conveying mechanism is arranged in the groove; electric push rods are fixed on both sides of the upper end of the workbench, and lifting blocks are fixed at one ends of the two electric push rods; a lifting plate is connected between the two lifting blocks, a mounting frame is fixed on one side of the upper end of the lifting plate, a conveying pipe penetrates through one side of the mounting frame, and the lower end of the conveying pipe penetrates through the lifting plate and extends to the lower end of the lifting plate; the lower end of the conveying pipe is slidably sleeved with a cover body, more than two springs are fixed at the upper end of the cover body, and the upper ends of the springs are fixed at the lower end of the lifting plate; the other side of the lifting plate penetrates through and is fixed with a bottle cap machine; the upper end of workstation all is fixed with the riser, and one side of two elevator all is equipped with stop gear.

2. The apparatus of claim 1, wherein the ammonium bifluoride and the potassium fluoride are produced as by-products in NF3 production, and the apparatus comprises: conveying mechanism is fixed with the bottle base more than two including installing the band conveyer in the recess on the band conveyer equidistant, can place the bottle in two of them bottle bases, and the upper end of one of them bottle corresponds each other with the lower extreme of the cover body, and the upper end of another bottle corresponds each other with the lower extreme of bottle lid machine.

3. The apparatus of claim 1, wherein the ammonium bifluoride and the potassium fluoride are produced as by-products in NF3 production, and the apparatus comprises: the limiting mechanism comprises limiting blocks arranged on one side of the two lifting blocks and limiting grooves arranged on the opposite sides of the two vertical plates, and the two limiting blocks are respectively arranged in the two limiting grooves.

4. The apparatus of claim 1, wherein the ammonium bifluoride and the potassium fluoride are produced as by-products in NF3 production, and the apparatus comprises: an electric valve is arranged on the conveying pipe.

5. The apparatus of claim 1, wherein the ammonium bifluoride and the potassium fluoride are produced as by-products in NF3 production, and the apparatus comprises: the bottle base is made of soft rubber materials, and the cover body is made of polypropylene materials.

6. A process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production is characterized in that: the method comprises the following steps:

s1, neutralizing and flushing the wastewater flowing out of the equipment: using KOH for neutralization, adjusting the pH value to be neutral, and adjusting the pH value to be 5-8;

s2, adjusting the pH value of the solution in the pH adjusting tank: controlling the pH to be more than 12, and completely precipitating Ni2+ in the solution;

s3, removing NH4+ in the solution: removing NH4+ in the solution under the conditions of strong alkaline environment and negative pressure heating, and carrying out vacuum treatment for 2h at 70 ℃;

s4, adjusting the pH value to be neutral, namely introducing tail gas containing hydrogen fluoride in the production into a spray tower, and spraying and absorbing the hydrogen fluoride to neutralize potassium hydroxide in a potassium fluoride solution;

s5, drying, filling and sealing, wherein spray drying is adopted, and after drying is finished, the mixture is introduced into a conveying pipe according to any one of claims 1 to 5 to be collected and sealed by a cover.

7. The process according to claim 6, characterized in that: the KF concentration in the solution was continuously measured in S1, and when the KF concentration reached 30%, the solution was transferred to a pH adjustment tank to adjust the pH.

8. The process according to claim 6, characterized in that: the precipitate formed in S2 is mainly hydroxide containing iron and nickel, and can be used together with the waste nickel slag in the previous step to prepare nickel sulfate through acid dissolution, iron removal, neutralization, crystallization and other processes.

9. The process according to claim 6, characterized in that: NH3 is also present in the vacuum off-gas in S3, and is absorbed by 70% waste sulfuric acid to become ammonium sulfate, preventing ammonia gas from escaping.

10. The process according to claim 6, characterized in that: in the spray drying in S5: the solution feeding concentration is 40%, the feeding temperature is 40 ℃, the air inlet temperature is 300 ℃, the flow is 400L/h, and the water content after spraying is less than 2%.

Technical Field

The invention relates to the field of fine chemical engineering, in particular to a device and a process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production.

Background

The waste water produced in the electrolysis production contains a large amount of ammonium bifluoride (ammonium fluoride), nickel fluoride, ferrous fluoride, sponge nickel, copper, iron and the like. These substances are toxic substances except iron. It is proved by people that Ni2+ (Ni) has stronger carcinogenic effect, F-also has stronger toxicity, China pays great attention to the aspect of environmental protection, and Ni2+ and F-are respectively listed as a first pollution control index and a second pollution control index (GB 8978-96), namely the highest allowable emission concentration of total nickel is 1.0mg/L, and the highest allowable emission concentration of fluoride is 10 mg/L. A series of researches on fluorine-containing wastewater at home and abroad are carried out, and good progress is made.

The current dangerous waste material that contains nickel fluorine can produce great pollution to the environment when handling, still need spend great cost during the processing, and current product adopts manual work cooperation machinery to carry out the installation of filling and bottle lid when the filling, and the cost of labor is higher, has the problem of filling inefficiency, for this reason, we have proposed one kind from device and the technology of by-product ammonium bifluoride and potassium fluoride in NF3 production to solve above-mentioned problem.

Disclosure of Invention

The invention aims to solve the defects in the prior art and provides a device and a process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production.

In order to achieve the purpose, the invention adopts the following technical scheme:

a device for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production comprises a workbench, wherein four corners of the lower end of the workbench are respectively fixed with a bearing rod; a groove is formed in the middle of the upper end of the workbench, and a conveying mechanism is arranged in the groove; electric push rods are fixed on both sides of the upper end of the workbench, and lifting blocks are fixed at one ends of the two electric push rods; a lifting plate is connected between the two lifting blocks, a mounting frame is fixed on one side of the upper end of the lifting plate, a conveying pipe penetrates through one side of the mounting frame, and the lower end of the conveying pipe penetrates through the lifting plate and extends to the lower end of the lifting plate; the lower end of the conveying pipe is slidably sleeved with a cover body, more than two springs are fixed at the upper end of the cover body, and the upper ends of the springs are fixed at the lower end of the lifting plate; the other side of the lifting plate penetrates through and is fixed with a bottle cap machine; the upper end of workstation all is fixed with the riser, and one side of two elevator all is equipped with stop gear.

Preferably, conveying mechanism is including installing the band conveyer in the recess, the equidistant bottle base more than two that is fixed with of band conveyer can place the bottle in two of them bottle bases, and the upper end of one of them bottle corresponds each other with the lower extreme of cover body, and the upper end of another bottle corresponds each other with the lower extreme of bottle lid machine.

Preferably, the limiting mechanism comprises limiting blocks arranged on one side of the two lifting blocks and limiting grooves arranged on the opposite sides of the two vertical plates, and the two limiting blocks are respectively arranged in the two limiting grooves.

Preferably, the delivery pipe is provided with an electric valve.

Preferably, the bottle base is made of soft rubber material, and the cover body is made of polypropylene material.

The invention also provides a process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production, which comprises the following steps:

s1, neutralizing and flushing the wastewater flowing out of the equipment: using KOH for neutralization, adjusting the pH value to be neutral, and adjusting the pH value to be 5-8;

s2, adjusting the pH value of the solution in the pH adjusting tank: controlling the pH to be more than 12, and completely precipitating Ni2+ in the solution;

s3, removing NH4+ in the solution: removing NH4+ in the solution under the conditions of strong alkaline environment and negative pressure heating, and completely removing NH4+ after vacuum treatment at 70 ℃ for 2 h;

s4, adjusting the pH value to be neutral, namely introducing tail gas containing hydrogen fluoride in the production into a spray tower, and spraying and absorbing the hydrogen fluoride to neutralize potassium hydroxide in a potassium fluoride solution;

and S5, drying, filling and sealing, namely spray drying is adopted, and after drying is finished, the mixture is introduced into a conveying pipe for collection and is covered and sealed.

Further, the KF concentration in the solution was continuously measured in S1, and when the KF concentration reached 30%, the solution was transferred to a pH adjusting tank to adjust the pH.

Further, the precipitate formed in S2 is mainly hydroxide containing iron and nickel, and may be used together with waste nickel slag in the previous step to prepare nickel sulfate through acid dissolution, iron removal, neutralization, crystallization and other processes.

Further, NH3 is also present in the vacuum offgas of S3, and is absorbed by 70% waste sulfuric acid to become ammonium sulfate, thereby preventing ammonia gas from overflowing.

Further, in the spray drying in S5: the solution feeding concentration is 40%, the feeding temperature is 40 ℃, the air inlet temperature is 300 ℃, the flow is 400L/h, and the water content after spraying is less than 2%.

Has the advantages that:

the invention can realize filling and bottle cap installation by intermittent movement of the bottle body, effectively saves labor cost, avoids dust from flying out, improves production efficiency, can eliminate dangerous waste containing nickel and fluorine, converts the dangerous waste into byproducts, reduces environmental pollution, can convert the dangerous waste which needs expensive treatment into the byproducts, and has certain economic benefit.

Drawings

FIG. 1 is a schematic diagram of the internal structure of an apparatus for producing ammonium bifluoride and potassium fluoride as by-products from NF3 production according to the present invention;

FIG. 2 is a front view of an apparatus for producing ammonium acid fluoride and potassium fluoride as by-products from NF3 according to the present invention;

FIG. 3 is a schematic structural diagram illustrating the operation state of an apparatus for producing ammonium bifluoride and potassium fluoride as by-products from NF3 production according to the present invention;

FIG. 4 is a top view of a lift plate of an apparatus for producing ammonium bifluoride and potassium fluoride as by-products from NF3 according to the present invention;

FIG. 5 is an enlarged view of the structure at the point A of the apparatus for producing ammonium bifluoride and potassium fluoride as by-products from NF3 according to the present invention;

in the figure: 1 workstation, 2 lifter plates, 3 elevator, 4 conveyer pipes, 5 mounting brackets, 6 bottle lid machines, 7 stopper, 8 spacing grooves, 9 risers, 10 electric putter, 11 bottles, 12 band conveyer, 13 bottle bases, 14 carrier bars, 15 covers the body, 16 springs, 17 electric valve.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.

Referring to fig. 1-5, a device of by-product ammonium bifluoride and potassium fluoride in NF3 production, including workstation 1, workstation 1's lower extreme four corners all is fixed with carrier bar 14, makes things convenient for the stable support of workstation 1, and workstation 1's upper end middle part is equipped with the recess, is equipped with conveying mechanism in the recess, and workstation 1's upper end both sides all are fixed with electric putter 10, and two electric putter 10's one end all is fixed with elevator 3, and two electric putter 10 drive two elevator 3 respectively through one end and reciprocate.

According to the invention, the lifting plate 2 is jointly fixed at one end of the two lifting blocks 3, the mounting frame 5 is fixed at one side of the upper end of the lifting plate 2, the conveying pipe 4 penetrates through one side of the mounting frame 5, the electric valve 17 is installed on the conveying pipe 4, the electric valve 17 is convenient to control the opening and closing of the conveying pipe 4, the product can be conveniently filled, the lower end of the conveying pipe 4 penetrates through the lifting plate 2 and extends to the lower end of the lifting plate 2, the cover body 15 is sleeved at the lower end of the conveying pipe 4 in a sliding mode, the cover body 15 is made of polypropylene materials, and the novel multifunctional electric lifting.

In the invention, more than two springs 16 are fixed at the upper end of the cover body 15, the upper ends of the springs 16 are fixed at the lower end of the lifting plate 2, when the cover body 15 abuts against the upper end of the bottle body 11, the cover body 15 can extrude the springs 16, so that the cover body 15 does not influence the continuous movement of the lifting plate 2 when abutting against the upper end of the bottle body 11, the other side of the upper end of the lifting plate 2 penetrates through and is fixed with the bottle cap covering machine 6, and the bottle cap covering machine 6 can carry out bottle cap installation work on the bottle body 11.

The upper end of the workbench 1 is fixed with a vertical plate 9, one side of each of the two lifting blocks 3 is provided with a limiting mechanism, and the limiting mechanisms are convenient for the lifting blocks 3 to stably move. Stop gear is including fixing the stopper 7 in two lifters 3 one sides respectively, and the relative one side of two risers 9 all is equipped with spacing groove 8, and two stoppers 7 are installed respectively in two spacing grooves 8, remove in spacing groove 8 through stopper 7.

In the invention, the conveying mechanism comprises a belt conveyor 12 arranged in the groove, the belt conveyor 12 is used for driving the bottle bodies 11 to move intermittently, so that the bottle bodies 11 are filled and the bottle caps on the bottle bodies 11 are installed, more than two bottle bases 13 are fixed on the belt conveyor 12 at equal intervals, and the bottle bases 13 are made of soft rubber materials and can deform so as to be convenient for adapting to the position change of the bottle bases on the belt conveyor 12.

In the invention, the bottle bodies 11 can be placed in the two bottle bases 13 at the same time, so that the stable placement of the bottle bodies 11 is ensured, the upper end of one bottle body 11 corresponds to the lower end of the cover body 15, the cover body 15 can conveniently cover the bottle bodies 11 to prevent powder from floating to influence the production environment during filling, the upper end of the other bottle body 11 corresponds to the lower end of the bottle capping machine 6, and the bottle capping machine 6 can conveniently mount a bottle cap on the upper end of the bottle body 11.

The invention also provides a process for producing ammonium bifluoride and potassium fluoride as byproducts in NF3 production, which comprises the following steps:

s1, neutralizing and flushing the wastewater flowing out of the equipment: the concentration of the ammonium bifluoride in the wastewater flowing out of the primary flushing equipment is lower, and if the wastewater is flushed by using the water circulation, the concentration of the ammonium bifluoride is higher and higher. Because ammonium bifluoride is strong corrosive substance, dissolves and washes equipment once more in aqueous and can cause the potential safety hazard, can cause equipment corrosion simultaneously, consequently uses KOH to carry out the neutralization, adjusts pH to neutral, utilizes the aqueous solution after the neutralization to carry out equipment washing, adjusts pH value control in this step at 5 ~ 8, and pH too high then makes the ammonia spill over easily, causes environmental pollution. Using KOH to neutralize NH4HF2 to generate KF continuously and circularly, measuring the concentration of a KF solution, and transferring the KF solution to a pH adjusting tank to adjust the pH value when the concentration of the KF reaches 30%;

s2, adjusting the pH value of the solution in the pH adjusting tank: the pH value is adjusted to remove metal ions in the solution, an alkaline environment is provided for next step of removing NH4+, and because the solution contains NH4+ and Ni2+, nickel ammonia complex ions can be formed in the alkaline environment, the pH value must be adjusted to be strong so as to destroy the complex ions to achieve the purpose of removing Ni2 +. Controlling the pH >12 enabled the Ni2+ in the solution to be fully precipitated. The formed precipitate is mainly hydroxide containing iron and nickel, and can be used for preparing nickel sulfate together with waste nickel slag in the previous working procedure through processes of acid dissolution, iron removal, neutralization, crystallization and the like;

s3, NH4+ removal: after metal ions in the solution are removed, the main component of the solution is a mixture of NH4F and KF, NH4+ in the solution is removed under the conditions of strong alkaline environment and negative pressure heating, NH4+ can be completely removed after vacuum treatment at 70 ℃ for 2h, and NH3 in vacuum tail gas is absorbed by 70% waste sulfuric acid generated in another product to become ammonium sulfate and prevent ammonia from overflowing;

s4, adjusting the pH value to be neutral: the solution after NH4+ removal is strong alkaline, the pH value needs to be adjusted to be neutral, in order to not introduce other impurities and save cost, tail gas containing hydrogen fluoride in production is introduced into a spray tower to be sprayed and absorbed to neutralize potassium hydroxide in a potassium fluoride solution, and when the solution is neutral, the solution is kept stand and filtered to enter a drying process;

s5, drying, filling and sealing: the drying can adopt crystallization drying or spray drying, the investment of crystallization drying equipment is small, but active potassium fluoride powder cannot be prepared, and the crystallization drying is not suitable for the preparation because the water absorption of the potassium fluoride is strong, the solution feeding concentration is 40%, the feeding temperature is 40 ℃, the air inlet temperature is 300 ℃, the flow is 400L/h, the water content after spraying is less than 2%, and the filling and sealing treatment are carried out after the preparation.

In the invention, after the treatment is finished, the conveying pipe 4 is used for conveying products, the bottles 11 are placed in the bottle base 13 on the belt conveyor 12 by a worker, the bottles 11 are driven by the belt conveyor 12 to move intermittently, so that the two bottles 11 can be respectively positioned at the lower ends of the bottle capper 6 and the cover body 15, the two electric push rods 10 respectively drive the two lifting blocks 3 through one end, the two lifting blocks 3 jointly drive the lifting plate 2 to move, so that the lifting plate 2 moves to drive the bottle capper 6 and the cover body 15 to move up and down, when the cover body 15 abuts against the upper end of the bottle 11, the cover body 15 extrudes the spring 16, so that the cover body 15 does not influence the continuous movement of the lifting plate 2 while abutting against the upper end of the bottle 11, the conveying pipe 4 is inserted into the bottle 11, the electric valve 17 is opened to convey the products into the bottle 11, and the bottle capper 6 can install a, drive 11 intermittent type nature removals of bottle through band conveyer 12, realize earlier the filling of bottle 11 and to the installation of bottle lid on the bottle 11, carry out material loading and unloading to bottle 11 through a staff, the effectual cost of labor that has saved, and improved production efficiency.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.