CN113213548B - Packaging method of ferrous chloride crystal - Google Patents
Packaging method of ferrous chloride crystal Download PDFInfo
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- CN113213548B CN113213548B CN202110522657.4A CN202110522657A CN113213548B CN 113213548 B CN113213548 B CN 113213548B CN 202110522657 A CN202110522657 A CN 202110522657A CN 113213548 B CN113213548 B CN 113213548B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
- B65B31/04—Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied
- B65B31/06—Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied the nozzle being arranged for insertion into, and withdrawal from, the mouth of a filled container and operating in conjunction with means for sealing the container mouth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B51/00—Devices for, or methods of, sealing or securing package folds or closures; Devices for gathering or twisting wrappers, or necks of bags
- B65B51/10—Applying or generating heat or pressure or combinations thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B51/00—Devices for, or methods of, sealing or securing package folds or closures; Devices for gathering or twisting wrappers, or necks of bags
- B65B51/10—Applying or generating heat or pressure or combinations thereof
- B65B2051/105—Heat seal temperature control
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Vacuum Packaging (AREA)
- Packages (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a packaging method of ferrous chloride crystals, which comprises the following steps: s1, adding reduced iron powder into ferrous chloride hot concentrated solution with Fe more than 15%, and adding a small amount of Fe in the ferrous chloride solution 3+ Reducing; s2, performing filter pressing while the solution is hot, cooling filtrate, crystallizing to separate ferrous chloride crystals, and performing centrifugal separation to obtain the ferrous chloride crystals; s3, crushing the bonded crystals into single grains with uniform particles by using a lump crusher; s4, using a hot-melt plastic packaging bag, placing a gas distributor connected with nitrogen at the bottom of the plastic bag, filling ferrous chloride crystals to the required weight while filling nitrogen, and taking out the packaging bag from the gas distribution plate; s5, vacuumizing, filling nitrogen and sealing the filled ferrous chloride by using an external vacuumizing machine. In the packaging process, the invention uses the technical means of breaking the agglomerate, gas distributor and filling while filling nitrogen to assist in vacuumizing to remove air existing between crystals, so as to prolong the preservation time of ferrous chloride crystals after packaging.
Description
Technical Field
The invention relates to a packaging technology of a compound, in particular to a preservation and packaging method of ferrous chloride crystals.
Background
The ferrous chloride crystal is exposed in the air in a large area, is easily oxidized after being contacted with oxygen in the air, and cannot easily meet the special requirements of the ferrous chloride crystal for the electronic industry. These industries require Fe in ferrous chloride crystals 3+ In industrial practical production, the standard is difficult to reach, and because high temperature is needed for evaporating and concentrating ferrous chloride liquid in the production process, ferrous is easy to oxidize in the process, so that crystals separated by crystallization are avoided from being entrained with a small amount of Fe 3+ At this time chloridizeFe in ferrous iron crystal 3+ Often greater than 0.1%, and in addition, the product is also easily and rapidly oxidized in the packaging process, and still easily oxidized by gaps between crystals and air in the package after packaging, and in addition, the long transportation time, when the product arrives at a customer, the green ferrous chloride crystals are already yellow, fe 3+ The index can not meet the requirements of customers, and oxidation always exists in the ferrous chloride production process, the packaging process and the transportation process, so that a preservation method of ferrous chloride crystals needs to be developed to prolong the shelf life of the product and meet the actual industrial requirements.
The preservation method of the ferrous chloride crystal is not disclosed in the patent, and the common vacuumizing and nitrogen filling preservation technology still has problems in the preservation of the ferrous chloride crystal. For example, in a direct vacuumizing packaging mode, the product is yellowing within one month, the ferrous chloride crystals are seriously bonded, a large solid structure, even a whole solid structure, is formed when the product is unsealed for use, and is inconvenient to pour, weigh, dissolve and the like.
Disclosure of Invention
The invention aims to provide a packaging method of ferrous chloride crystals, which can prevent the ferrous chloride crystals from being oxidized by air in the packaging and transportation processes and prolong the preservation time of the ferrous chloride crystals.
In order to solve the technical problems, the adopted technical scheme is as follows:
a method for packaging ferrous chloride crystals, comprising the steps of:
s1, adding reduced iron powder into ferrous chloride hot concentrated solution with Fe more than 15%, and adding a small amount of Fe in the ferrous chloride solution 3+ Reducing;
s2, performing hot press filtration, cooling filtrate, crystallizing to separate ferrous chloride crystals, and separating the ferrous chloride crystals from liquid through a centrifugal machine to obtain ferrous chloride crystals;
s3, crushing the bonded crystals into single grains with uniform particles by using a lump crusher;
s4, using a hot-melt plastic packaging bag, placing a gas distributor connected with nitrogen at the bottom of the plastic bag, filling ferrous chloride crystals to the required weight while filling the nitrogen, and taking out the gas distributor from the packaging bag;
s5, vacuumizing, filling nitrogen and sealing the filled ferrous chloride by using an external vacuumizing machine.
Further, the higher the concentration of ferrous chloride, the higher the crystal precipitation temperature, the less the amount of the reduced iron powder needs to be added, the faster the reaction, the temperature is controlled to be 60-90 ℃, and the mass ratio of the reduced iron powder to the solution is as follows: 0.5-1:1000. The process can effectively reduce Fe in ferrous chloride solution 3+ The content of the ferrous chloride is achieved, and the purpose of purifying the ferrous chloride is achieved.
Furthermore, in the operation process, the concentration of the ferrous chloride solution is higher, so that the press filtration work needs to be completed quickly, the ferrous chloride crystals separated out by natural cooling and excessive reduced iron powder are prevented from being separated out of a solution system together, and the ferrous chloride concentrated solution after press filtration is cooled and crystallized, and the purer ferrous chloride crystals can be obtained through centrifugal operation.
Furthermore, the lump breaker is mainly used for scattering the block crystals which are formed to be bonded in the crystallization and centrifugation processes, eliminating the liquid and air which are wrapped in the lump breaker, and facilitating the subsequent vacuumizing process to remove the air, water vapor and the like as much as possible.
Further, the gas distributor is placed at the bottom of the plastic bag, nitrogen is firstly filled, air in the plastic bag is replaced by nitrogen, the ferrous chloride crystals are filled while nitrogen is filled, the gas distributor is continuously lifted upwards according to the filling condition of the ferrous chloride crystals, the gas distributor is buried below the ferrous chloride crystals by about 10cm to facilitate the subsequent taking out of the gas distributor, the operation can fully discharge air among grain gaps out of the plastic bag, the phenomenon that only one process step of vacuumizing is used for discharging air among ferrous chloride crystals is avoided, and residual air slowly oxidizes ferrous chloride due to incomplete air discharging is avoided.
Further, after the gas distributor is taken out, the outer vacuumizing machine is rapidly used for vacuumizing, filling nitrogen and sealing. When vacuumizing, ensuring that the reading of the pressure gauge is between-0.08 and-0.1 MPa, and keeping for 3-5 seconds, so that the air in the package is pumped out as much as possible; when nitrogen is filled, the packaging bag is slightly bulged, so that the sealing bag is prevented from being punctured by sharp objects, and the preservation failure of ferrous chloride crystals is prevented; the temperature of the hot-melt seal is 60-80 ℃, and alkaline water is needed to be used for checking whether the package opening leaks air or not after the hot-melt seal is finished, so that the tightness of ferrous chloride crystal package is ensured.
In the invention, a small amount of Fe contained in the solution is reduced by improving the production process 3+ Reduction to ensure that the ferrous chloride crystals are free of Fe prior to packaging 3+ In the state, the technical means of breaking the agglomerate, gas distributor and filling while filling nitrogen are used for assisting in vacuumizing to remove air existing between the crystals, so that the preservation time of the ferrous chloride crystals after packaging is prolonged, the ferrous chloride crystals are in a loose state when unpacking and using, and the using experience of customers is greatly improved.
Detailed Description
Example 1
A method for packaging ferrous chloride crystals, comprising the steps of:
s1, adding 0.8kg of reduced iron powder into 1 ton of ferrous chloride hot concentrated solution with 18.6% of Fe and 80 ℃ to obtain 0.63% Fe in ferrous chloride solution 3+ Restoring to undetected state;
s2, hot press filtration, cooling filtrate to below 25 ℃ and crystallizing to separate ferrous chloride crystals, and separating the ferrous chloride crystals from the liquid by a centrifugal machine to obtain 0.62 ton of ferrous chloride crystals;
s3, crushing the bonded crystals into uniform single grains by using a lump crusher;
s4, using a hot-fusible polypropylene/polyethylene composite film packaging bag, placing a gas distributor connected with nitrogen at the bottom of the packaging bag, filling ferrous chloride crystals to 20kg while filling nitrogen, and taking out the packaging bag from a gas distribution plate;
s5, vacuumizing the packaging bag filled with the ferrous chloride to-0.1 MPa by using an external vacuumizing machine, maintaining for 5S, and filling nitrogen gas until the packaging bag slightly bulges and is subjected to hot melting and sealing at the temperature of 70 ℃. The seal was checked for leakage by alkaline water.
The packed ferrous chloride crystals are placed in a warehouse at normal temperature, and are opened at different times to sample and check the conditions of products, and the results are shown in the following table:
example 2
A method for packaging ferrous chloride crystals, comprising the steps of:
s1, adding 1kg of reduced iron powder into 1 ton of ferrous chloride hot concentrated solution with Fe of 16.5% and temperature of 60 ℃ to obtain 0.42% Fe in ferrous chloride solution 3+ Restoring to undetected state;
s2, hot press filtration, filtrate cooling to below 15 ℃ and crystallization to separate ferrous chloride crystals, and separating the ferrous chloride crystals from the liquid by a centrifugal machine to obtain 0.47 ton of ferrous chloride crystals;
s3, crushing the bonded crystals into uniform single grains by using a lump crusher;
s4, using a hot-fusible polypropylene/polyethylene composite film packaging bag, placing a gas distributor connected with nitrogen at the bottom of the packaging bag, filling ferrous chloride crystals to 40kg while filling nitrogen, and taking out the gas distribution plate from the packaging bag;
s5, vacuumizing the packaging bag filled with the ferrous chloride to-0.1 MPa by using an external vacuumizing machine, maintaining for 5S, and filling nitrogen to slightly bulge, wherein the temperature of the hot melting sealing is 60 ℃. The seal was checked for leakage by alkaline water.
The packed ferrous chloride crystals are placed in a warehouse at normal temperature, and are opened at different times to sample and check the conditions of products, and the results are shown in the following table:
example 3
A method for packaging ferrous chloride crystals, comprising the steps of:
s1, adding 0.5kg of reduced iron powder into 1 ton of ferrous chloride hot concentrated solution with 20.1% of Fe and 90 ℃ to obtain 0.74% of Fe in ferrous chloride solution 3+ Restoring to undetected state;
s2, hot press filtration, cooling filtrate to below 20 ℃ and crystallizing to separate ferrous chloride crystals, and separating the ferrous chloride crystals from the liquid by a centrifugal machine to obtain 0.69 ton of ferrous chloride crystals;
s3, crushing the bonded crystals into uniform single grains by using a lump crusher;
s4, using a hot-fusible polypropylene/polyethylene composite film packaging bag, placing a gas distributor connected with nitrogen at the bottom of the packaging bag, filling ferrous chloride crystals to 25kg while filling nitrogen, and taking out the packaging bag from a gas distribution plate;
s5, vacuumizing the packaging bag filled with the ferrous chloride to-0.8 MPa by using an external vacuumizing machine, maintaining for 5S, and filling nitrogen gas until the packaging bag slightly bulges and is subjected to hot melting and sealing at the temperature of 80 ℃. The seal was checked for leakage by alkaline water.
The packed ferrous chloride crystals are placed in a warehouse at normal temperature, and are opened at different times to sample and check the conditions of products, and the results are shown in the following table:
comparative example 1
The ferrous chloride crystals produced in the step S2 of the example 1 are packaged by a plastic bag and then are simply wrapped and sealed.
Comparative example 2
And (3) packaging the ferrous chloride crystals produced in the step S2 in the example 1 by using a plastic bag, vacuumizing, and sealing by hot melting.
Comparative example 3
And (3) packaging the ferrous chloride crystals produced in the step S2 in the example 1 by using a plastic bag, vacuumizing, flushing nitrogen, and sealing by hot melting.
The ferrous chloride crystals packaged in the manner of comparative example were placed in a warehouse under the same conditions as in the examples, and the packaged samples were opened at different times to examine the condition of the products, and the results are shown in the following table:
from the results of the above examples and comparative examples, it can be derived that: the oxidation speed of ferrous chloride can be relatively slowed down by using the common fresh-keeping modes of vacuumizing, nitrogen charging and sealed packaging, but the preservation effect still cannot meet the requirement of ferrous chloride to Fe for the electronic industry 3+ < 0.1% of the requirements. Through the improvement of the packaging technology, the air and water vapor existing between the crystals are removed as much as possible by the technical means of breaking the agglomerate, using the gas distributor and filling while filling with nitrogen, so that the ferrous chloride crystals after sealed packaging can be stably maintained for more than one year.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.
Claims (7)
1. A method for packaging ferrous chloride crystals, comprising the steps of:
s1, adding reduced iron powder into ferrous chloride hot concentrated solution with Fe more than 15%, and adding a small amount of Fe in the ferrous chloride solution 3+ Reducing;
s2, performing hot press filtration, cooling filtrate, crystallizing to separate ferrous chloride crystals, and separating the ferrous chloride crystals from liquid through a centrifugal machine to obtain ferrous chloride crystals;
s3, crushing the bonded crystals into single grains with uniform particles by using a lump crusher;
s4, using a hot-melt plastic packaging bag, placing a gas distributor connected with nitrogen at the bottom of the plastic bag, filling ferrous chloride crystals to the required weight while filling nitrogen, and taking out the packaging bag from the gas distribution plate;
s5, vacuumizing, filling nitrogen and sealing the filled ferrous chloride by using an external vacuumizing machine.
2. The method for packaging ferrous chloride crystals as set forth in claim 1, wherein: the mass ratio of the addition amount of the reduced iron powder to the solution in the S1 is 0.5-1:1000.
3. The method for packaging ferrous chloride crystals as set forth in claim 1, wherein: and S4, continuously lifting the gas distributor upwards according to the filling condition of the ferrous chloride crystal, so that the gas distributor is buried below the solid particles by 10cm, and the gas distributor can be conveniently taken out later.
4. The method for packaging ferrous chloride crystals as set forth in claim 1, wherein: in S5, the vacuumizing condition is as follows: the reading of the pressure gauge is between-0.08 and-0.1 MPa, and the pressure gauge is kept for 3-5S.
5. The method for packaging ferrous chloride crystals as set forth in claim 4, wherein: s5, the temperature of the hot-melt sealing is as follows: 60-80 ℃.
6. The method for packaging ferrous chloride crystals as set forth in claim 5, wherein: and after S5, checking whether the package mouth leaks or not by using alkaline water after the hot-melt sealing is completed.
7. The method for packaging ferrous chloride crystals as set forth in claim 1, wherein: the temperature of the ferrous chloride hot concentrated solution in the S1 is 60-90 ℃.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1224378A (en) * | 1968-04-26 | 1971-03-10 | Alberta Res Council | A method for converting particulate ferrous chloride to iron |
| JPH10272301A (en) * | 1997-03-31 | 1998-10-13 | Nittetsu Mining Co Ltd | Method for treating ferrous compound-containing hydrochloric acid waste solution |
| CN203345231U (en) * | 2013-05-22 | 2013-12-18 | 上海垚远科技发展有限公司 | Feedback type nitrogen-filled vacuum package machine |
| CN110950389A (en) * | 2019-12-27 | 2020-04-03 | 斯瑞尔环境科技股份有限公司 | Production process of granular ferrous chloride dihydrate |
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
| CN112062164A (en) * | 2020-08-25 | 2020-12-11 | 斯瑞尔环境科技股份有限公司 | Production method of reagent-grade ferric trichloride |
-
2021
- 2021-05-13 CN CN202110522657.4A patent/CN113213548B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1224378A (en) * | 1968-04-26 | 1971-03-10 | Alberta Res Council | A method for converting particulate ferrous chloride to iron |
| JPH10272301A (en) * | 1997-03-31 | 1998-10-13 | Nittetsu Mining Co Ltd | Method for treating ferrous compound-containing hydrochloric acid waste solution |
| CN203345231U (en) * | 2013-05-22 | 2013-12-18 | 上海垚远科技发展有限公司 | Feedback type nitrogen-filled vacuum package machine |
| CN110980833A (en) * | 2019-12-16 | 2020-04-10 | 斯瑞尔环境科技股份有限公司 | Preparation method of electronic-grade ferrous chloride |
| CN110950389A (en) * | 2019-12-27 | 2020-04-03 | 斯瑞尔环境科技股份有限公司 | Production process of granular ferrous chloride dihydrate |
| CN112062164A (en) * | 2020-08-25 | 2020-12-11 | 斯瑞尔环境科技股份有限公司 | Production method of reagent-grade ferric trichloride |
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