CN107200308A - A kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature - Google Patents
A kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature Download PDFInfo
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- CN107200308A CN107200308A CN201710311913.9A CN201710311913A CN107200308A CN 107200308 A CN107200308 A CN 107200308A CN 201710311913 A CN201710311913 A CN 201710311913A CN 107200308 A CN107200308 A CN 107200308A
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- potassium peroxydisulfate
- purification
- potassium
- recrystallization
- crystal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
- C01B15/06—Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
- C01B15/08—Peroxysulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to fine chemistry industry and technical field of analytical chemistry, a kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature is disclosed.Methods described is：Sodium chloride solution is heated to 50 DEG C, then potassium peroxydisulfate stirring and dissolving is added to hypersaturated state, crystallized being placed in after the supersaturated potassium persulfate solution sealing of gained under temperature conditionss below freezing, taken out when crystal is no longer separated out, abandoning supernatant, crystal is cleaned with 4 DEG C of pure water, is then dried at a temperature of 50 DEG C, obtains potassium peroxydisulfate after purification.4 DEG C of the common temperature of recrystallization is to effectively reduced to below freezing by the present invention using reduction of the sodium chloride to aqueous solution freezing point, loss amount of the potassium peroxydisulfate in recrystallization process is effectively reduced, so that the rate of recovery of potassium peroxydisulfate is greatly improved.
Description
Technical field
The invention belongs to fine chemistry industry and technical field of analytical chemistry, and in particular to one kind is recrystallized purified based on low temperature
The method of potassium sulfate.
Background technology
Potassium peroxydisulfate is a kind of quite varied chemical reagent of purposes, can be used as oxidant, preservative, fabric bleaching agent,
Polymerization accelerant, thermal initiator, analytical reagent and photographic chemical, are also used in terms of medicine, dyestuff.Although however, domestic right
The production requirement of potassium peroxydisulfate performs standard《Chemical reagent potassium persulfate (potassium peroxydisulfate)》(GB/T 641-2011), still
Many domestic potassium peroxydisulfates still there are problems that not reaching this, for example, according to《The alkaline mistake of the measure of water quality total nitrogen
Potassium sulfate ultraviolet spectrophotometry》(HJ 636-2012) surveys water quality index total nitrogen, and digestion agent is prepared using domestic potassium peroxydisulfate
When, often have that blank value is too high and the measure that causes domestic potassium peroxydisulfate to cannot be used for water quality index total nitrogen.Domestic many prisons
The domestic potassium peroxydisulfate quality dissatisfactions of all Zeng Yinwei such as survey station, laboratory and cause determination of total nitrogen content to fail, for the solution of the problem
Certainly mode mainly has 2 kinds at present：One is the potassium peroxydisulfate of the external production of direct purchase, and its quality can meet measure demand, but take
With higher, by taking 500g/ bottles of potassium peroxydisulfate as an example, the price of both Sigma companies and Chinese medicines group is respectively 1014 yuan and 31
Member, the former is nearly 33 times of the latter；Two be to carry out repeated recrystallize purification to domestic potassium peroxydisulfate in laboratory, meets and determines need
Ask and reuse, but under commonly recrystallization purification operations, the rate of recovery is very low, the time of this operation, human cost sum are high
In corresponding economic benefit.Therefore, how improving the rate of recovery of potassium peroxydisulfate purifying, improving the product quality of domestic potassium peroxydisulfate
It is the big major issue of one currently faced.
The quality of domestic potassium peroxydisulfate is improved, top priority is that research understands that it influences the main component of determination of total nitrogen content.
According to the production technology of potassium peroxydisulfate, it is known that its one of raw material that chemically reacts is ammonium hydrogen sulfate, and one of intermediate reaction product is sulphur
Sour ammonium, so very likely there is the residual of nitrogen；Found according to literature survey, domestic potassium peroxydisulfate blank value it is too high and
Our early stages by the measure to wherein ammonia nitrogen, total nitrogen content, can determine the quality problem of domestic potassium peroxydisulfate mainly its
Middle ammonia nitrogen, total nitrogen content severe overweight, so it is not up to standard to directly results in domestic potassium peroxydisulfate quality, have impact on water quality total nitrogen and refer to
Target is determined.After the reason for sour potassium quality of the clear domestic persulfuric acid of research is not up to standard, domestic many scientific research personnel, which have studied, to be carried
The method of the sour potassium quality of high persulfuric acid, mainly purifies domestic potassium peroxydisulfate by recrystallizing.This method is although simple to operate easy
OK, but its rate of recovery is very low.
Domestic potassium peroxydisulfate product quality is not up to standard in the urgent need to improving its quality, domestic production manufacturer non-counterweight knot so far
Brilliant purifying technique is applied, and its one of the main reasons is that the rate of recovery is very low, is insufficient for its corresponding economic benefit.For
This, the rate of recovery of the domestic potassium peroxydisulfate purifying of raising produces the improvement of the production technology of the potassium peroxydisulfate of high-quality to China with pushing away
Wide application pole is necessary.
The content of the invention
In place of the shortcoming and defect existed for above prior art, low temperature is based on it is an object of the invention to provide one kind
The method of recrystallization purification potassium peroxydisulfate.The rate of recovery and product quality to improve potassium peroxydisulfate.
The object of the invention is achieved through the following technical solutions：
A kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature, is comprised the following steps：
Sodium chloride solution is heated to 50 DEG C, potassium peroxydisulfate stirring and dissolving is then added to hypersaturated state, by gained mistake
Crystallization under the conditions of freezing point (0 DEG C) temperature below is placed in after the sealing of saturation potassium persulfate solution, takes out, abandons when crystal is no longer separated out
Supernatant is removed, crystal is cleaned with 4 DEG C of pure water, is then dried at a temperature of 50 DEG C, obtains potassium peroxydisulfate after purification.
Preferably, the mass fraction of the sodium chloride solution is 0.002%~0.5%.
Preferably, the number of times that crystal is cleaned with 4 DEG C of pure water is 3 times.
The present invention principle be：The solubility of potassium peroxydisulfate has close ties with temperature；Therefore, in this theoretical foundation
On, by properly increasing temperature during dissolving to improve supersaturated solution concentration, create cryogenic conditions when recrystallizing to reduce
Loss amount in recrystallization process, can both have been purified using recrystallization this method advantage simple and easy to apply, while can with gram
The low inferior position of the clothes recrystallization purification rate of recovery.Low temperature recrystallization can be created to the reduction of aqueous solution freezing point using sodium chloride
Condition, solubility during reduction potassium peroxydisulfate recrystallization；In addition, potassium peroxydisulfate can be because of high temperature failure, to ensure not lose at 60 DEG C
The supersaturation concentration tried one's best while effect when improving dissolving, we select 50 DEG C as solution temperature.In addition, low-temperature pure water is rinsed
Also a part of impurity can be taken away, is that this can be 3 times with pure water rinsing to potassium peroxydisulfate recrystallization crystal.
The method of purification of the present invention has the following advantages that and beneficial effect：
(1) reduction using sodium chloride to aqueous solution freezing point, freezing point is to effectively reduced to by 4 DEG C of the common temperature of recrystallization
(0 DEG C) below, is effectively reduced loss amount of the potassium peroxydisulfate in recrystallization process, so that the recovery of potassium peroxydisulfate is greatly improved
Rate；
(2) the inventive method dissolving potassium peroxydisulfate and the temperature dried are 50 DEG C, can make supersaturated solution during dissolving
Concentration try one's best it is high, rate of drying is improved, while also ensuring that potassium peroxydisulfate, not because pyrolytic fails, improves whole recrystallization and carried
The pure rate of recovery and efficiency；
(3) cryogenic conditions when being recrystallized by the raising and creation of solution temperature, can make the recovery recrystallized for the first time
Rate maintains more than 84%, and the rate of recovery of second of recrystallization is more than 70%, by low temperature recrystallization operation twice, is obtained
The total nitrogen content of potassium sulfate meets the potassium peroxydisulfate of GB/T 641-2011 production standards；Its recycled in its entirety rate is than common recrystallization
The overall recovery of method of purification will be higher by more than 14%, and remarkable in economical benefits is improved.
Brief description of the drawings
Fig. 1 is recrystallized under times conditions to be different in embodiment, the variation diagram of total nitrogen content in 1# potassium peroxydisulfates；
Fig. 2 is under different recrystallization times conditions in embodiment, 1# potassium peroxydisulfates recrystallizes the variation diagram of the rate of recovery；
Fig. 3 is recrystallized under times conditions to be different in embodiment, the variation diagram of total nitrogen content in 2# potassium peroxydisulfates；
Fig. 4 is under different recrystallization times conditions in embodiment, 2# potassium peroxydisulfates recrystallizes the variation diagram of the rate of recovery；
Fig. 5 is recrystallized under times conditions to be different in embodiment, the variation diagram of total nitrogen content in 3# potassium peroxydisulfates；
Fig. 6 is under different recrystallization times conditions in embodiment, 3# potassium peroxydisulfates recrystallizes the variation diagram of the rate of recovery.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment
Three kinds of potassium peroxydisulfates (label 1#, 2#, 3#) are subjected to recrystallization and remove total nitrogen and ammonia nitrogen：
(1) measure 150.0mL pure water, 0.002%~0.5% mass sodium chloride into 250mL beakers, in 50 DEG C of water-baths
Heated in pot, rallentando add potassium peroxydisulfate product (about 25g or so), and be stirred continuously with glass bar, when solution was
During saturation state, stop stirring and taking out；
(2) it is rapid that beaker mouthful is strictly sealed with PE films, beaker and solution therein are transferred to 4 DEG C of refrigerators of ﹣
Stand, the extraneous factor interference such as do not allow solution vibrated in the process is taken out when crystal is no longer separated out；
(3) supernatant of crystallization is discarded, the crystal of precipitation 4 DEG C of pure water rinsings 3 times, then crystal is transferred to 250mL
In beaker；
(4) crystal is put into 50 DEG C of baking ovens and be dried, rear taking-up to be dried；
(5) first time recrystallization crystal is continued to dissolve by heating in 50 DEG C of water-baths to hypersaturated state, repeat step
(2)、(3)、(4)；
(6) crystal obtained by step (5) is put into wide-mouth Brown Glass Brown glass bottles and jars only, sealing preserve.
Under difference recrystallization times condition, the change of total nitrogen content in three kinds of domestic potassium peroxydisulfates (label 1#, 2#, 3#)
Change and《Chemical reagent potassium persulfate (potassium peroxydisulfate)》(GB/T 641-2011) is distinguished total nitrogen required standard line in reagent
As shown in Fig. 1, Fig. 3, Fig. 5；Under difference recrystallization times condition, three kinds of domestic potassium peroxydisulfates (label 1#, 2#, 3#) recrystallize back
The situation of change of yield and the contrast difference with common pure water recrystallization (being added without sodium chloride, recrystallization temperature is 4 DEG C) result
As shown in Fig. 2, Fig. 4, Fig. 6.From Fig. 1, Fig. 3, Fig. 5, method of purification total nitrogen removal efficiency of the invention is all very high；And pass through
After 2 recrystallizations, the total nitrogen content of three kinds of domestic potassium peroxydisulfates can meet the production standard of its execution.By Fig. 2, Fig. 4, Fig. 6
Understand, recrystallization, the rate of recovery of second of recrystallization are respectively 85%~88%, 70% to the potassium peroxydisulfate of the present embodiment for the first time
~79%；The secondary recrystallization rate of recovery will improve more than 14% respectively than the rate of recovery of common recrystallization operation, fully show
Low temperature recrystallizes the advantage of condition.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (3)
1. a kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature, it is characterised in that comprise the following steps：
Sodium chloride solution is heated to 50 DEG C, potassium peroxydisulfate stirring and dissolving is then added to hypersaturated state, by gained supersaturation
It is placed under temperature conditionss below freezing and crystallizes after potassium persulfate solution sealing, is taken out when crystal is no longer separated out, abandoning supernatant,
Crystal is cleaned with 4 DEG C of pure water, is then dried at a temperature of 50 DEG C, obtains potassium peroxydisulfate after purification.
2. a kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature according to claim 1, it is characterised in that：It is described
The mass fraction of sodium chloride solution is 0.002%~0.5%.
3. a kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature according to claim 1, it is characterised in that：It is described
The number of times that crystal is cleaned with 4 DEG C of pure water is 3 times.
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| CN201710311913.9A CN107200308A (en) | 2017-05-05 | 2017-05-05 | A kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature |
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| CN201710311913.9A CN107200308A (en) | 2017-05-05 | 2017-05-05 | A kind of method that purification potassium peroxydisulfate is recrystallized based on low temperature |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551490A (en) * | 2020-11-24 | 2021-03-26 | 河北冀衡集团有限公司威武分公司 | Preparation method of ammonium persulfate crystals |
| CN116119623A (en) * | 2023-01-29 | 2023-05-16 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105546141A (en) * | 2016-01-22 | 2016-05-04 | 王志法 | Counter weight liquid for electric control gate and automatic gate |
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2017
- 2017-05-05 CN CN201710311913.9A patent/CN107200308A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105546141A (en) * | 2016-01-22 | 2016-05-04 | 王志法 | Counter weight liquid for electric control gate and automatic gate |
Non-Patent Citations (1)
| Title |
|---|
| 赵新鲜: "过硫酸钾提纯方法对总氮测定结果的影响及控制", 《新疆水利》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551490A (en) * | 2020-11-24 | 2021-03-26 | 河北冀衡集团有限公司威武分公司 | Preparation method of ammonium persulfate crystals |
| CN116119623A (en) * | 2023-01-29 | 2023-05-16 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
| CN116119623B (en) * | 2023-01-29 | 2023-08-15 | 西陇科学股份有限公司 | Production method of environment-friendly high-purity potassium persulfate |
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Application publication date: 20170926 |