CN110668471B - Purification production method of environment-friendly potassium persulfate - Google Patents
Purification production method of environment-friendly potassium persulfate Download PDFInfo
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Abstract
The invention discloses a purification production method of environment-friendly potassium persulfate, which comprises the following steps: step 1, adding industrial potassium persulfate raw materials into pure water, stirring and soaking, and stirring and dissolving the soaked potassium persulfate raw materials by using the pure water; step 2, after the raw materials are completely dissolved, carrying out heat preservation, precipitation and filtration, cooling the solution, adding a proper amount of absolute ethyl alcohol, and stirring for full crystallization; step 3, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, and carrying out secondary recrystallization after the primary crystals are completely dissolved by pure water; and 4, carrying out crystal drying treatment on the obtained crystals meeting the requirements, and finally obtaining the environment-friendly potassium persulfate product. The anhydrous ethanol is added to participate in the crystallization process, so that the impurities which are not easy to remove by water are effectively removed under the condition of not introducing the impurities, the product meets the requirement of environmental protection level, and the defects of the existing production method are overcome.
Description
Technical Field
The invention relates to the technical field of chemical reagent production, in particular to a method for purifying and producing environment-friendly potassium persulfate.
Background
Potassium persulfate is an inorganic compound, white crystal, odorless, and mainly used as bleaching agent, strong oxidant, photographic chemicals, analytical reagent, polymerization accelerator, etc. When the potassium persulfate is used as a strong oxidant, the potassium persulfate is a key reagent for measuring total nitrogen in alkaline potassium persulfate digestion ultraviolet spectrophotometry, so that the purity of the potassium persulfate is required to be high enough, and the nitrogen content of the potassium persulfate is required to be low enough.
Meanwhile, due to the enhancement of the environmental protection management, for potassium persulfate serving as a high-purity chemical reagent, enterprises respond to national policies and also put forward environmental protection level requirements on potassium persulfate products, namely the purity of the environmental protection level potassium persulfate is required to reach at least 99.5 wt%, the total nitrogen content is not higher than 0.0005 wt%, the iron content is not higher than 0.0002 wt%, and the heavy metal content is not higher than 0.001 wt%. The preparation method commonly adopted in the industry of environmental protection level potassium persulfate at present is as follows: the method takes Ethylene Diamine Tetraacetic Acid (EDTA) as a chelating agent, generates a water-soluble complex with impurities in analytically pure potassium persulfate, removes the impurities in the potassium persulfate through recrystallization, and then obtains environment-friendly potassium persulfate, however, the method has a great defect that the impurities in the water-soluble Ethylene Diamine Tetraacetic Acid (EDTA) are introduced, so that the purity of the potassium persulfate is insufficient, the total nitrogen content is high, the main indexes of the potassium persulfate cannot meet the requirement of the environment-friendly level, the potassium persulfate needs to be purified and treated with high cost at the later stage, and the production cost of enterprises is too high.
Chinese patent CN105565278A discloses a preparation method of high-purity low-nitrogen potassium persulfate, which comprises the following steps: 1. adding distilled water into a pressure container, and then adding potassium persulfate to carry out reduced pressure distillation; 2. pouring the solution into a crystallizing tank for cooling and crystallizing, and then washing crystals; 3. adding distilled water to dissolve the crystals, filtering, distilling under reduced pressure, cooling the crystals again, washing and drying in vacuum to obtain the product. In the method, the crystals are purified and purified mainly by cooling and crystallizing and washing the crystals by using ice water and ethanol, although no new impurities are introduced, the method can only clean and remove impurities on the surfaces of the crystals and cannot remove impurities in the crystals, namely, ammonia ions and iron ions contained in a solution can enter the crystals and be wrapped when potassium persulfate is cooled and crystallized, and only the ammonia ions and the iron ions on the surfaces of the crystals can be removed when the crystals are washed at the later stage, so that the impurity content of the final product cannot exceed the standard because the crystals cannot be washed in the crystals. Although the recrystallization mode can effectively purify the water-soluble impurities, the recrystallization purification medium is mainly pure water which can only effectively remove the water-soluble impurities and can not remove the water-insoluble organic matters and partial inorganic matters, such as nitrogen-containing organic matters and iron ions, so that the final crystal still contains more impurities, the nitrogen content and the iron content can not be reduced to ideal values, the method is not an optimal mode, in addition, the potassium persulfate can obviously decompose at the temperature of over 52 ℃, for industrial production, the decomposition of the potassium persulfate below 50 ℃ can be ignored, the purity of the potassium persulfate can not be influenced, and therefore, the yield of the complicated reduced pressure distillation mode is not high, and only the production cost can be increased.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the method for purifying and producing the environmental-friendly potassium persulfate is provided, and the anhydrous ethanol is added to participate in the crystallization process, so that the impurities outside and inside the crystal are effectively removed under the conditions of not introducing the impurities and ensuring low-cost production, the final product meets the environmental-friendly requirement, and the defects of the existing production method are overcome.
The technical scheme adopted by the invention is as follows: the method for purifying and producing the environmental-friendly potassium persulfate is characterized by comprising the following steps of:
step 1, adding an industrial potassium persulfate raw material into a closed container, adding a proper amount of pure water, stirring and soaking, performing dehydration treatment after complete soaking, stirring and dissolving the soaked potassium persulfate raw material with pure water, and controlling the dissolving temperature to be below 50 ℃;
step 2, after the raw materials are completely dissolved, carrying out heat preservation and precipitation, then filtering the solution, removing insoluble impurities, cooling the solution, controlling the cooling temperature at 10-30 ℃, adding a proper amount of absolute ethyl alcohol after cooling for a certain time, and then stirring for fully crystallizing;
step 3, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, completely dissolving the primary crystals with pure water, carrying out secondary recrystallization, then dehydrating to obtain secondary crystals, and carrying out repeated crystallization until crystals meeting the requirements are obtained;
and 4, carrying out crystal drying treatment on the obtained crystals meeting the requirements, wherein the crystal drying temperature is below 50 ℃, and finally obtaining the environment-friendly potassium persulfate product.
In the method, the key point is step 2, and in step 2, the key point is the addition of absolute ethyl alcohol, namely absolute ethyl alcohol is added after the solution is cooled for a certain time, when crystallization begins in the solution, the absolute ethyl alcohol can absorb impurities such as organic matters, metal ions and the like in the solution and is miscible with water, so that the crystallization process of potassium persulfate is accelerated while impurities are removed, the crystallization time is shortened, so that the impurities entrapped in the crystals are very few when the solution is crystallized, the purity of the obtained crystals is extremely high, some organic matters (including organic nitrogen) which cannot be removed by pure water can be removed, part of metal ions (such as iron ions) and part of water can also be removed by the absolute ethyl alcohol, and all indexes of the prepared potassium persulfate crystals, particularly the indexes of nitrogen content and iron content, meet the environmental protection level requirement, overcomes the problems of the prior preparation method.
It is worth pointing out that in the method, only absolute ethyl alcohol can be used, or only ethyl alcohol with extremely high purity and containing very little impurity and water can not be used, even the ethyl alcohol solution with the mass fraction reaching 95% can not be used, the inventor summarizes after a plurality of experiments, the inventor finds that when the solution is cooled and crystallized, the solution mainly comprises partial crystallization and saturated potassium persulfate solution, at the moment, the absolute ethyl alcohol is added, impurities such as organic matters in the saturated potassium persulfate solution are firstly dissolved in the absolute ethyl alcohol and then partially mixed and dissolved with the ethyl alcohol, thereby promoting the crystallization of the solution while removing impurities, if the ethyl alcohol solution is used, the water in the ethyl alcohol solution firstly dissolves the crystallized crystals and then dissolves the impurities and then crystallizes when the saturated potassium persulfate solution is formed, although the ethyl alcohol solution can achieve the purpose of removing the impurities, however, the crystallization of the solution can not be promoted, and the crystallization process is also negatively influenced, so that the crystallization of the potassium persulfate is not facilitated, and therefore, the effect of the absolute ethyl alcohol cannot be achieved by adding the ethanol solution.
Furthermore, although the method introduces organic anhydrous ethanol, the boiling point of the anhydrous ethanol is low, and trace anhydrous ethanol wrapped by the dehydrated product can be completely volatilized in the concentration and crystal drying processes, so that the purity of the anhydrous ethanol cannot be influenced.
Furthermore, in the invention, the purpose of the step 1 is mainly to pretreat the raw material potassium persulfate to remove impurities attached to the surface of the potassium persulfate crystal, but the potassium persulfate is also dissolved in water, so that the added water during soaking is not excessive, excessive water can consume excessive potassium persulfate, at the same time, the soaked water is not too little, otherwise the raw material cannot be soaked sufficiently, the effect of pre-impurity removal is poor, and the subsequent treatment process is influenced, and after a plurality of tests of the inventor, the mass ratio of the pure water used for soaking to the industrial potassium persulfate raw material is proper between (1-2) and 5, which can be 1:5, 2:5, 1.4:5, 1.5:5 and 1.6:5, and can also be 1.2:5 and 1.3:5, and the specific ratio can be selected according to actual use.
Further, when the soaking water is enough, in order to ensure that the potassium persulfate can be fully soaked, the soaking time is a key factor, and after a plurality of tests of the inventor, the soaking time needs to be more than 20 hours to ensure that the potassium persulfate can be fully soaked. Of course, the soaking time is related to the amount of the potassium persulfate raw material, the soaking time is longer when the amount is larger, the soaking time is shorter when the amount is smaller, the soaking time can be lower than 20h for small-scale or experimental potassium persulfate purification, but for industrial production, the soaking time is generally about 50kg for one-time potassium persulfate purification production, and the soaking time is not shorter than 20h for full soaking of the potassium persulfate raw material on the scale.
Further, in step 2 of the method, after the raw materials are fully dissolved by pure water, the raw materials need to be kept warm for a certain time for precipitation so as to remove insoluble impurities, in order to remove the insoluble impurities as much as possible and balance the production time, the heat-preservation precipitation time of the method is preferably 1-3h, when the solution amount is small, the heat-preservation precipitation time can be properly shortened, 1h can be selected, and otherwise, 3h can be selected.
Further, in step 2, in order to fully utilize the anhydrous ethanol, the mass ratio of the anhydrous ethanol to the industrial potassium persulfate raw material is (1-2): 5.
Preferably, in step 3, after the secondary crystal is obtained, the secondary crystal is subjected to a crystal baking treatment as it is. That is, although a satisfactory product can be obtained by performing crystallization twice, it is needless to say that recrystallization for the third time, recrystallization for the fourth time, and the like can be performed, but since recrystallization for the third time and recrystallization for the subsequent time have little influence on the purification effect and the cost performance is not high, it is preferable to perform crystallization twice.
Further, in step 4, in order to perform a sufficient crystal baking treatment, water and ethanol in the crystals were evaporated, and the crystal baking time was 7 hours or more.
In addition, in the method of the present invention, the soaked water and the crystallized water need to be treated separately, for example: the soaked water is generally further refined to obtain analytically pure or reagent-grade potassium persulfate products, and the crystallized water is distilled at low temperature to recover ethanol and the like. The cooling time in step 2 is generally not specifically limited, and is determined basically according to field observation, that is, when obvious crystallization is observed in the solution, absolute ethyl alcohol can be added, and accordingly, when the crystallization is judged to be complete, and according to experience, when 30-40 wt% of crystallization is precipitated in the solution, the crystallization is complete, and then dehydration treatment can be performed.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the invention provides a purification production method of environment-friendly potassium persulfate, which is characterized in that anhydrous ethanol is added to participate in the crystallization process, impurities outside and inside a crystal are effectively removed under the condition of not introducing the impurities, and water-insoluble organic matters and part of metal ions are particularly removed, so that the finally obtained product meets the environment-friendly requirement, and the problem that the potassium persulfate produced by the existing production method cannot meet the environment-friendly requirement is solved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The purification production method of the environmental protection grade potassium persulfate comprises the following steps:
step 1, adding 50kg of industrial potassium persulfate raw material into a closed container, then adding 12kg of pure water for complete soaking, and continuously stirring, wherein the soaking time is 30 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked potassium persulfate raw material by using pure water, controlling the dissolving temperature to be below 50 ℃, and stirring to fully dissolve the potassium persulfate raw material;
step 3, after complete dissolution, filtering the solution after heat preservation and precipitation for 1h, and then cooling and crystallizing the solution, wherein the cooling temperature is controlled at 20 ℃;
step 4, after the solution is cooled for a certain time, obviously crystallizing and separating out the solution, at the moment, adding 20kg of absolute ethyl alcohol, and stirring for fully crystallizing;
step 5, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, carrying out additional treatment on the dehydrated solution, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 6, carrying out crystal drying treatment on the secondary crystals in a vacuum drying oven, wherein the crystal drying temperature is 48 ℃, and the crystal drying time is 8 hours, thus obtaining the product finally.
Example 2
The purification production method of the environmental protection grade potassium persulfate comprises the following steps:
step 1, adding 50kg of industrial potassium persulfate raw material into a closed container, then adding 20kg of pure water for complete soaking, and continuously stirring, wherein the soaking time is 20 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked potassium persulfate raw material by using pure water, controlling the dissolving temperature to be below 50 ℃, and stirring to fully dissolve the potassium persulfate raw material;
step 3, after complete dissolution, filtering the solution after heat preservation and precipitation for 4 hours, and then cooling and crystallizing the solution, wherein the cooling temperature is controlled at 10 ℃;
step 4, after the solution is cooled for a certain time, obviously crystallizing and separating out the solution, at the moment, adding 20kg of absolute ethyl alcohol, and stirring for fully crystallizing;
step 5, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, carrying out additional treatment on the dehydrated solution, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 6, carrying out crystal drying treatment on the secondary crystals in a vacuum drying oven, wherein the crystal drying temperature is 47 ℃, and the crystal drying time is 10 hours, thus obtaining the product finally.
Example 3
The purification production method of the environmental protection grade potassium persulfate comprises the following steps:
step 1, adding 50kg of industrial potassium persulfate raw material into a closed container, then adding 14kg of pure water for complete soaking, and continuously stirring, wherein the soaking time is 24 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked potassium persulfate raw material by using pure water, controlling the dissolving temperature to be below 50 ℃, and stirring to fully dissolve the potassium persulfate raw material;
step 3, after complete dissolution, filtering the solution after heat preservation and precipitation for 2 hours, and then cooling and crystallizing the solution, wherein the cooling temperature is controlled at 20 ℃;
step 4, after the solution is cooled for a certain time, obviously crystallizing and separating out the solution, at the moment, adding 14kg of absolute ethyl alcohol, and stirring for fully crystallizing;
step 5, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, carrying out additional treatment on the dehydrated solution, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 6, carrying out crystal drying treatment on the secondary crystals in a vacuum drying oven, wherein the crystal drying temperature is 45 ℃, and the crystal drying time is 10 hours, thus obtaining the product finally.
Example 4
The purification production method of the environmental protection grade potassium persulfate comprises the following steps:
step 1, adding 50kg of industrial potassium persulfate raw material into a closed container, then adding 15kg of pure water for complete soaking, and continuously stirring, wherein the soaking time is 24 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked potassium persulfate raw material by using pure water, controlling the dissolving temperature to be below 50 ℃, and stirring to fully dissolve the potassium persulfate raw material;
step 3, after complete dissolution, filtering the solution after heat preservation and precipitation for 2 hours, and then cooling and crystallizing the solution, wherein the cooling temperature is controlled at 30 ℃;
step 4, after the solution is cooled for a certain time, obviously crystallizing and separating out the solution, at the moment, adding 14kg of absolute ethyl alcohol, and stirring for fully crystallizing;
step 5, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, carrying out additional treatment on the dehydrated solution, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 6, carrying out crystal drying treatment on the secondary crystals in a vacuum drying oven, wherein the crystal drying temperature is 47 ℃, and the crystal drying time is 8 hours, thus obtaining the product finally.
Example 5
The purification production method of the environmental protection grade potassium persulfate comprises the following steps:
step 1, adding 50kg of industrial potassium persulfate raw material into a closed container, then adding 17kg of pure water for complete soaking, and continuously stirring, wherein the soaking time is 25 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked potassium persulfate raw material by using pure water, controlling the dissolving temperature to be below 50 ℃, and stirring to fully dissolve the potassium persulfate raw material;
step 3, after complete dissolution, filtering the solution after heat preservation and precipitation for 2 hours, and then cooling and crystallizing the solution, wherein the cooling temperature is controlled at 20 ℃;
step 4, after the solution is cooled for a certain time, obvious crystallization is separated out in the solution, at the moment, 13kg of absolute ethyl alcohol is added, and the solution is stirred for full crystallization;
step 5, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, carrying out additional treatment on the dehydrated solution, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 6, carrying out crystal drying treatment on the secondary crystals in a vacuum drying oven, wherein the crystal drying temperature is 40 ℃, and the crystal drying time is 11 hours, thus obtaining the product finally.
The test data for the products obtained in examples 1 to 5 above are shown in the following table:
TABLE 1 raw assay data for samples run Nos. 1-5 (examples 1-5)
Sampling date: 2019.03.20 room temperature: 16 deg.C
The results shown in table 1 indicate that the products obtained in the above 5 examples all meet the environmental protection level requirements, which indicates that the purification production method of environmental protection level potassium persulfate provided by the present invention is successful, and can be used for producing environmental protection level potassium persulfate, thereby solving the problem that the existing production method can not meet the requirements of environmental protection level products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. The method for purifying and producing the environmental-friendly potassium persulfate is characterized by comprising the following steps of:
step 1, adding an industrial potassium persulfate raw material into a closed container, adding a proper amount of pure water, stirring and soaking, performing dehydration treatment after complete soaking, stirring and dissolving the soaked potassium persulfate raw material with pure water, and controlling the dissolving temperature to be below 50 ℃;
step 2, after the raw materials are completely dissolved, carrying out heat preservation and precipitation, then filtering the solution, removing insoluble impurities, cooling the solution, controlling the cooling temperature at 10-30 ℃, cooling for a certain time until obvious crystallization is separated out in the solution, then adding absolute ethyl alcohol, and then stirring for full crystallization; the mass ratio of the absolute ethyl alcohol to the industrial potassium persulfate raw material is (1-2) to 5;
step 3, after complete crystallization, carrying out dehydration treatment to obtain primary crystals, completely dissolving the primary crystals with pure water, carrying out secondary recrystallization, then dehydrating to obtain secondary crystals, and carrying out repeated crystallization until crystals meeting the requirements are obtained;
and 4, carrying out crystal drying treatment on the obtained crystals meeting the requirements, wherein the crystal drying temperature is below 50 ℃, and finally obtaining the environment-friendly potassium persulfate product.
2. The process for producing potassium persulfate according to claim 1, wherein the ratio of the amount of pure water used for the immersion to the amount of raw material potassium persulfate in the industrial process in step 1 is (1-2): 5.
3. The process for purifying and producing environmental protection grade potassium persulfate as claimed in claim 1, wherein in the step 1, the soaking time is more than 20 h.
4. The process for purifying and producing environmental protection grade potassium persulfate as claimed in claim 1, wherein in the step 2, the heat preservation and precipitation time is 1-3 h.
5. The method for purifying and producing environmental-friendly potassium persulfate according to claim 1, wherein in the step 3, after the secondary crystal is obtained, the secondary crystal is directly subjected to crystal baking treatment.
6. The method for purifying and producing environmental protection grade potassium persulfate as claimed in claim 1, wherein in the step 4, the crystal drying time is more than 7 h.
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| CN112683823A (en) * | 2020-12-17 | 2021-04-20 | 飞鸣科学仪器（武汉）有限公司 | Detection reagent for detecting total nitrogen content in wastewater and preparation method |
| CN117427365B (en) * | 2023-12-20 | 2024-03-15 | 福建铭麟科技有限公司 | Potassium persulfate preparation technology and preparation device |
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| CA2669834A1 (en) * | 2006-11-16 | 2008-05-22 | Albemarle Netherlands B.V. | Purification of molybdenum technical oxide |
| CN102050764B (en) * | 2010-11-27 | 2012-05-23 | 吉林众鑫化工集团有限公司 | Method for purifying sodium hydroxyethyl sulphonate |
| CN105016306A (en) * | 2014-04-23 | 2015-11-04 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
| CN104176748A (en) * | 2014-08-15 | 2014-12-03 | 广州衡创测试技术服务有限公司 | Method for purifying potassium persulfate |
| CN105565278A (en) * | 2014-10-14 | 2016-05-11 | 天津市光复科技发展有限公司 | Preparation method of high-purity low-nitrogen potassium persulfate |
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