CN109160525B - Adsorption purification method of industrial potassium chloride - Google Patents
Adsorption purification method of industrial potassium chloride Download PDFInfo
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Abstract
The invention relates to the field of impurity removal of industrial potassium chloride, and provides an adsorption purification method of industrial potassium chloride. Adding potassium carbonate and potassium hydroxide into industrial potassium chloride, fully reacting and precipitating for 10-14h, and filtering to obtain a first filtrate; adding an adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption into the first filtrate for adsorption for 10-14h to obtain a liquid to be separated; and filtering and separating the liquid to be separated to obtain a second filtrate, and drying the second filtrate to obtain the solid food potassium chloride. The novel technology is a novel technology which utilizes an adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption to adsorb and purify industrial potassium chloride to prepare food-grade potassium chloride, can remove harmful substances such as heavy metals and the like while removing amine, and further prepares the food-grade potassium chloride; the preparation process has low energy consumption, high efficiency, simple process, low cost and easy industrial production.
Description
Technical Field
The invention relates to the field of impurity removal of industrial potassium chloride, and particularly relates to an adsorption purification method of industrial potassium chloride.
Background
The food-grade potassium chloride is mainly prepared from agricultural-grade potassium chloride and industrial-grade potassium chloride, the market price of the industrial potassium chloride is 1950 yuan/t, and the product value is low. Because potassium chloride is mostly produced by a flotation method, the product contains a trace amount of flotation agents. From the global market, along with the improvement of living standard of people, the demand of products such as low-sodium salt products, seasonings and the like is rapidly increased, which drives the stable increase of the consumption of upstream food-grade ingredients such as potassium chloride and the like. Therefore, the food-grade potassium chloride product has great production potential, the market price is stable at 5700-7000 yuan/t, and the added value of the product is high.
Aiming at industrial potassium chloride products (containing residual flotation agents and overproof lead-arsenic heavy metal ions) prepared by a flotation method in salt lake chemical industry, the food potassium chloride is prepared by calcining potassium chloride in the traditional industry, and the process is complex, the energy consumption is high, and the cost is high. Or the industrial potassium chloride is sequentially subjected to macroporous resin adsorption, activated carbon adsorption, concentration crystallization and other processes to prepare the food potassium chloride, the process is complex, and the purification effect is poor.
Disclosure of Invention
The invention aims to provide an adsorption and purification method of industrial potassium chloride, which is simple and can remove heavy metals and organic matters in the industrial potassium chloride by a one-step method so as to reach the national standard of food potassium chloride.
The embodiment of the invention is realized by the following steps:
an adsorption purification method of industrial potassium chloride, which comprises the following steps: adding potassium carbonate and potassium hydroxide into industrial potassium chloride, fully reacting and precipitating for 10-14h, and filtering to obtain a first filtrate;
adding an adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption into the first filtrate for adsorption for 10-14h to obtain a liquid to be separated;
and filtering and separating the liquid to be separated to obtain a second filtrate, and drying the second filtrate to obtain the solid food potassium chloride.
The beneficial effects of the embodiment of the invention include:
in the embodiment, the adsorption and purification of the industrial potassium chloride by using the adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption to prepare the food-grade potassium chloride is a new process, which is different from the conventional method. When industrial potassium chloride is adsorbed, amine is removed, and meanwhile, harmful substances such as heavy metals and the like can be removed, so that a novel technology for preparing food-grade potassium chloride is further provided; the preparation process has low energy consumption, high efficiency, simple process, low cost and easy industrial production.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for adsorption purification of industrial potassium chloride according to the embodiment of the present invention will be specifically described below.
An adsorption purification method of industrial potassium chloride, which comprises the following steps:
s1, adding potassium carbonate and potassium hydroxide into industrial potassium chloride, fully reacting and precipitating for 10-14h, and filtering to obtain a first filtrate;
the main impurity ions contained in industrial potassium chloride are calcium and magnesium, such as: the potassium carbonate is added to react with calcium ions in industrial potassium chloride to form calcium carbonate precipitates, and the potassium hydroxide is added to react with magnesium ions in the industrial potassium chloride to generate magnesium hydroxide precipitates, so that the aim of removing calcium and magnesium impurities is fulfilled.
S2, adding an adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption into the first filtrate for adsorption for 10-14h to obtain a liquid to be separated;
the industrial potassium chloride contains a large amount of organic matters and heavy metal ions besides a large amount of impurity ions, such as: lead and arsenic which exceed the standards. In this embodiment, the adsorbent is added to the first filtrate, and the adsorbent can adsorb polar substances and nonpolar substances at the same time, thereby further removing organic substances and heavy metals in industrial potassium chloride in one step.
Stirring once every 20-40min in the adsorption process, and standing after stirring. Stirring can make adsorbent and first filtrate mix better evenly, and the stewing can make adsorbent and first filtrate better carry out the reaction.
The adsorbent in this embodiment may be a combination of a polar adsorbent and a non-polar adsorbent, or may be a single component by having both polar adsorption and non-polar adsorption.
Specifically, in this embodiment, the adsorbent may be, for example, zeolite and activated carbon at a mass ratio of 1:1, or the adsorbent may also be activated bone carbon. Wherein the activated bone charcoal is prepared by mixing crushed animal waste bone with an activating agent and soaking for 12-20 h; and then activating for 60-90 min at the temperature of 500-850 ℃ to obtain an activated material, directly washing the activated material with water until the pH value is 6-8, and drying to obtain the catalyst.
Specifically, the preparation method of the activated bone charcoal comprises the following steps:
s201, airing: drying the waste animal bones until the water content is 5-15%.
S202, crushing: animal waste bones are crushed according to the process requirement.
S203, impregnation of an activating agent: mixing the crushed animal waste bone with activating agent and soaking for 12-20 h. Wherein the mass ratio of the activator to the waste animal bones is 1.5-3:1, and the activator is phosphoric acid. The mass ratio of phosphoric acid to the animal waste bone is 2-3:1, the concentration of phosphoric acid is 50-85%, the animal waste bone and an activating agent are soaked, the activating agent has a dehydration effect and a swelling effect on carbon-containing organic matters and can be fully contacted with the waste bone, the waste bone is activated at a certain temperature (different temperature ranges required by different activating agents), the activating agent interacts with materials at a high temperature in the process, carbon elements in the organic matters are fixed (such as phosphoric acid), and the oxidized amorphous parts are corroded to form micropores and mesopores, so that the specific surface area is greatly increased, and the waste bone is activated into an adsorbing material with strong adsorption capacity.
S204, high-temperature activation: and then activating for 60-90 min at the temperature of 500-650 ℃ to obtain the activated material.
Specifically, heating to a first activation temperature at a heating rate of 15-25 ℃/min, activating for 20-30min, heating to a second activation temperature at a heating rate of 5-10 ℃/min, and continuing to activate for 40-60 min; wherein the first activation temperature is 500-550 ℃, and the second activation temperature is 600-650 ℃; the first activation temperature is lower than the second activation temperature.
In the application, the immersed animal waste bone is subjected to high-temperature activation through the stepped activation temperature, the temperature is increased to a first activation temperature at the temperature increase speed of 15-25 ℃/min, the animal waste bone is activated at the first activation temperature, preheating and carbonization of the animal waste bone are realized, meanwhile, an activating agent attached to the surface of the animal waste bone after immersion is partially evaporated by high temperature to form gas, at the moment, part of the gas enters the inside of the carbon material along with carbonization of the animal waste bone, and after activation at the first activation temperature is finished, the temperature is increased to a second activation temperature at the temperature increase speed of 5-10 ℃/min, so that the temperature increase rate when the temperature is increased to the second activation temperature is obviously lower than that when the temperature is increased to the first activation temperature, because the temperature is increased to the first activation temperature at a higher temperature increase speed for activation, the animal waste bone is carbonized as soon as possible, and then the temperature is raised to the second activation temperature at a lower temperature raising speed, so that the carbonized animal waste bone is continuously opened in a continuous activation state, and is easy to react with gas generated by the high temperature of the activating agent, and further, the pores are continuously enlarged and develop to the depth. As the activation reaction is continuously carried out, the activation temperature is increased to the second activation temperature, new unsaturated carbon atoms or active points are exposed on the surface of the microcrystal, and then the new active points can react with other molecules of the activation gas, so that the uneven combustion on the surface of the microcrystal continuously causes the formation of new pores, and the activation effect is better.
S205, cooling: cooling the activated material to room temperature at a cooling speed of 8-11 ℃/min. The temperature is reduced and cooled at a specific temperature reduction speed, so that the contact time of the activated material and air is reduced, the porous structure on the surface of the activated material is shaped in the temperature reduction process, the activated material is not easily influenced by oxygen, carbon dioxide or water vapor in the air, and the property of the activated material is favorably kept.
S206, water washing: directly washing the activated material with water until the pH value is 6-8.
The active material is directly washed by water instead of acid, so that the surface structure of the active material is protected to the maximum extent, and meanwhile, the active agent which does not react with the animal waste aggregate can be recycled in the washing process by water.
S207, drying: drying at 100-120 deg.C for 8-12h to obtain activated bone charcoal, and removing water on the surface of the activated bone charcoal by drying.
After drying, the mass percent of the mass of the activated bone charcoal to the mass of the oven dry raw material is calculatedThe yield of the activated bone charcoal can be obtained, and the specific surface area of the activated bone charcoal obtained by the method is 200-500m2The methylene blue adsorption value is 30-130 mg/g.
The specific surface area of the activated bone charcoal was measured by a Tristar3000analyzer (Micromeritics, USA). The specific surface area was calculated according to the Brunaue-Emmett-Teller (BET) equation. The method for measuring the methylene blue adsorption value comprises the following steps: the methylene blue adsorption value is measured according to the national standard GB/T12496.10-1999 test method of wooden activated carbon: determination of methylene blue adsorption value.
The method takes the waste animal bones as raw materials, and phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride as an activating agent to prepare the activated bone charcoal with large specific surface area and high adsorption performance; is beneficial to realizing the resource utilization of various animal waste bones and saving resources such as wood, coal, coconut shell and the like. The prepared various animal bone-based activated bone charcoals can be used for replacing part of the traditional activated carbon products; the preparation process does not need inert gas protection, the process is simple, and the industrial production is easy to realize.
S3, filtering and separating the liquid to be separated to obtain a second filtrate, and drying the second filtrate to obtain the solid food potassium chloride.
In the solid food potassium chloride, As is 0-1.94mg/kg, Pb is 0-4.68mg/kg, and NH4 +In trace amounts. The determination of arsenic content in potassium chloride adopts PF6-2 Atomic Fluorescence Spectrometer (AFS); the content of lead and sodium is measured by TAS-990AFGSuper Flame Atomic Absorption spectrometer (Flame Atomic Absorption Spectroscopy, FAAS); the NH4+ content of potassium chloride was determined using a Cleverchem Anna fully automated batch chemical Analyzer (ADA).
In the embodiment, the adsorption and purification of the industrial potassium chloride by using the adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption to prepare the food-grade potassium chloride is a new process, which is different from the conventional method. The novel technology for preparing the food-grade potassium chloride by using the activated bone charcoal which is low in price, good in adsorption effect, safe and environment-friendly as the adsorbent to adsorb the adsorbent, and removing the amine and harmful substances such as heavy metal at the same time; the preparation process has low energy consumption, high efficiency, simple process, low cost and easy industrial production.
The process for the adsorption purification of industrial potassium chloride according to the present invention is further illustrated below with reference to examples.
Example 1
The embodiment provides an adsorption purification method of industrial potassium chloride, which comprises the following steps:
firstly, preparing active aggregate (phosphoric acid activated waste pig bone charcoal adsorbing material): 20g of waste pig bone material was weighed out and mixed with 50g of phosphoric acid (85% strength) activator and immersed for 15 hours. And (3) putting the completely soaked materials into a box-type resistance furnace, heating to 550 ℃ at the speed of 20 ℃/min, activating for 60min, naturally cooling to room temperature, taking out, washing for 5 times, filtering, drying at 110 ℃ for 10h, taking out, grinding, sieving, and filling the prepared powdery activated pig bone charcoal adsorbing material sample into a sample bag for later use.
Weighing 5g of the above activated bone charcoal, adding into 100ml of saturated industrial potassium chloride treated with potassium carbonate and potassium hydroxide, stirring once every 30 minutes, adsorbing for 12 hours, filtering and drying after adsorption to obtain the final product of potassium chloride, and measuring the yield and arsenic, lead and NH4 in the potassium chloride+The content of (a).
Examples 2 to 5
Examples 2 to 5 provide a method for adsorption purification of industrial potassium chloride, which is substantially the same as example 1, and 2 to 5 are activated bone charcoal prepared by phosphoric acid activation, except that the preparation process of the activated aggregate is different:
in example 2, the temperature was raised to 500 ℃ at 20 ℃/min for activation for 20min, and then raised to 600 ℃ at a temperature rise rate of 10 ℃/min for further activation for 40 min.
In example 3, after activation, the activated material was cooled to room temperature at a cooling rate of 10 ℃/min.
In example 4, the temperature was raised to 500 ℃ at 20 ℃/min for activation for 20min, and then raised to 600 ℃ at a temperature rise rate of 10 ℃/min for further activation for 40 min; and then cooling the activated material to room temperature at a cooling speed of 10 ℃/min.
In example 5, the raw material was a waste bovine bone material.
Example 6
The embodiment provides an adsorption purification method of industrial potassium chloride, which comprises the following steps:
weighing 2.5g of zeolite and 2.5g of activated carbon, adding the zeolite and the activated carbon into 100ml of saturated industrial potassium chloride treated by potassium carbonate and potassium hydroxide, stirring once every 30 minutes, adsorbing for 12 hours, filtering and drying after the adsorption is finished to obtain a finished product of potassium chloride, and measuring the yield and arsenic, lead and NH4 in the finished product of potassium chloride+The content of (a).
The activated bone charcoal obtained in the middle of the above examples 1-5 was tested for yield, specific surface area and methylene blue adsorption, and the test results are shown in Table 1.
TABLE 1 activated bone charcoal product Properties of examples 1-5
Arsenic, lead and NH4 of examples 1-6 above+The test results of the content of (b) are shown in table 2.
TABLE 2 arsenic, lead and NH4 of examples 1-6+Test results of the content of
Comparative experiment
Influence of one or more adsorbents on adsorption effect
Comparative example 1: the phosphoric acid activated bone charcoal in example 1 was replaced with activated charcoal as an organic adsorbent;
comparative example 2: the phosphate activated bone in example 1 was replaced with commercial bovine bone char;
comparative example 3: the phosphate activated bone in example 1 was replaced with chitosan as a heavy metal adsorbent;
comparative example 4: the phosphate-activated bone in example 1 was replaced with a phosphate-activated bone prepared by mixing, as a mass ratio, 1:1 with chitosan;
comparative example 5: the phosphate active bone in the embodiment 1 is replaced by lignin, wherein the existing literature shows that the lignin has adsorption effect on organic matters and heavy metal ions;
comparative example 6: the phosphate activated bone in example 1 was replaced with zeolite as a heavy metal adsorbent; taking the products obtained in the comparative examples 1-6 as an adsorbent, adding 100ml of saturated industrial potassium chloride treated by potassium carbonate and potassium hydroxide, stirring once every 30 minutes, adsorbing for 12 hours, filtering and drying after adsorption to obtain the finished product of potassium chloride, and measuring the yield and arsenic, lead and NH in the finished product of potassium chloride4 +The content of (a). The test results are shown in table 3. Arsenic, lead and NH of comparative examples 1-64 +The test results of the content of (b) are shown in table 3.
TABLE 3 arsenic, lead and NH4 of comparative examples 1-6+Test results of the content of
As shown in the table, examples 1 and 6 both reach the national standard of food-grade potassium chloride, while heavy metal ions of lead and arsenic in comparative examples 1 and 4 do not reach the national standard; heavy metal ions of lead, arsenic and NH in comparative examples 2, 3 and 54 +All do not meet the national standard, NH in comparative example 64 +The national standard is not met. This indicates that different adsorbents have a greater effect on the adsorption effect.
Secondly, the influence of the activated bone carbon prepared by different activating agents on the adsorption effect
Comparative example 7: the activator phosphoric acid in example 1 was replaced with pure potassium hydroxide (prepared as a 50% strength aqueous solution);
comparative example 8: the activator phosphoric acid in example 1 was replaced with pure zinc chloride (prepared as a 60% strength aqueous solution);
comparative example 9: the activator phosphoric acid in example 1 was replaced with pure magnesium chloride (prepared as a 60% strength aqueous solution) and mixed with the activator;
using the products obtained in comparative examples 7 to 9 as adsorbents, potassium carbonate and hydrogen were addedStirring once every 30 minutes in 100ml of saturated industrial potassium chloride treated by potassium oxide, adsorbing for 12 hours, filtering and drying after adsorption to obtain the finished product of potassium chloride, and measuring the yield and arsenic, lead and NH in the finished product4 +The content of (a). The test results are shown in table 4.
TABLE 4 arsenic, lead and NH4 of comparative examples 7-9+Test results of the content of
As shown in the table, heavy metal ions of lead, arsenic and NH in comparative examples 7, 8 and 94 +The difference of the activated bone charcoal obtained by different activators is obvious.
In summary, in the embodiment, the adsorption purification of the industrial potassium chloride by using the adsorbent capable of simultaneously performing the polar adsorption and the non-polar adsorption to prepare the food-grade potassium chloride is a new process, which is different from the conventional method. In particular, the activated bone charcoal prepared by a specific method is used as an adsorbent, has low price, good adsorption effect, safety and environmental protection, can adsorb industrial potassium chloride, remove amine, and simultaneously can remove harmful substances such as heavy metal and the like, thereby further preparing a new technology of food-grade potassium chloride; the preparation process has low energy consumption, high efficiency, simple process, low cost and easy industrial production.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. An adsorption purification method of industrial potassium chloride is characterized by comprising the following steps: adding potassium carbonate and potassium hydroxide into industrial potassium chloride, fully reacting and precipitating for 10-14h, and filtering to obtain a first filtrate;
adding an adsorbent capable of simultaneously performing polar adsorption and nonpolar adsorption into the first filtrate for adsorption for 10-14h to obtain a liquid to be separated;
filtering and separating the liquid to be separated to obtain a second filtrate, and drying the second filtrate to obtain solid food potassium chloride;
the adsorbent is activated bone charcoal which is obtained by activating phosphoric acid as an activating agent;
the activated bone charcoal is prepared by mixing crushed animal waste bones with an activating agent and soaking for 12-20 h; then activating for 60-90 min at the temperature of 500-650 ℃ to obtain an activated material, cooling the activated material to room temperature at the cooling speed of 8-11 ℃/min, then directly washing the activated material with water until the pH value is 6-8, and drying to obtain the active material; the mass ratio of the activating agent to the waste animal bones is 2-3: 1;
wherein, the activation for 60-90 min at the temperature of 500-650 ℃ to obtain the activated material comprises the following steps: activating at the first activation temperature for 20-30min, heating to the second activation temperature at a temperature rise rate of 5-10 deg.C/min, and activating for 40-60 min; wherein the first activation temperature is 500-550 ℃, and the second activation temperature is 600-650 ℃; the first activation temperature is lower than the second activation temperature.
2. The method for adsorbing and purifying industrial potassium chloride according to claim 1, wherein the industrial potassium chloride is stirred once every 20-40min during the adsorption process, and is left to stand after being stirred.
3. The method for adsorbing and purifying industrial potassium chloride As claimed in claim 1, wherein the solid food potassium chloride contains 0-1.94mg/kg of As, 0-4.68mg/kg of Pb and NH4 +In trace amounts.
4. The method for adsorbing and purifying industrial potassium chloride as claimed in claim 1, wherein the activated bone charcoal is obtained by directly washing the activating material with water to pH 6-8 and then drying at 100-120 ℃ for 8-12 h.
5. The method for adsorbing and purifying industrial potassium chloride according to claim 1, wherein the animal waste bone powder is air-dried until the moisture content is 5 to 15% before the animal waste bone powder is pulverized.
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| CN101721974A (en) * | 2010-01-14 | 2010-06-09 | 新疆大学 | Method for preparing animal bone matrix activated carbon adsorbent |
| CN105060315A (en) * | 2015-09-06 | 2015-11-18 | 华陆工程科技有限责任公司 | Method for producing food-grade potassium chloride by adopting adsorption process |
| CN107617416A (en) * | 2017-09-28 | 2018-01-23 | 浙江海洋大学 | A kind of preparation method of adsorbable heavy metal anglers bone biological carbon materials |
| CN108423692A (en) * | 2018-03-22 | 2018-08-21 | 安徽泰格生物技术股份有限公司 | With the method for production of vitamin C abraum salt purification sodium chloride |
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| CN101721974A (en) * | 2010-01-14 | 2010-06-09 | 新疆大学 | Method for preparing animal bone matrix activated carbon adsorbent |
| CN105060315A (en) * | 2015-09-06 | 2015-11-18 | 华陆工程科技有限责任公司 | Method for producing food-grade potassium chloride by adopting adsorption process |
| CN107617416A (en) * | 2017-09-28 | 2018-01-23 | 浙江海洋大学 | A kind of preparation method of adsorbable heavy metal anglers bone biological carbon materials |
| CN108423692A (en) * | 2018-03-22 | 2018-08-21 | 安徽泰格生物技术股份有限公司 | With the method for production of vitamin C abraum salt purification sodium chloride |
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