CN101229922B - Method for abstracting potassium from straw by microwave technique - Google Patents
Method for abstracting potassium from straw by microwave technique Download PDFInfo
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- CN101229922B CN101229922B CN200710048312XA CN200710048312A CN101229922B CN 101229922 B CN101229922 B CN 101229922B CN 200710048312X A CN200710048312X A CN 200710048312XA CN 200710048312 A CN200710048312 A CN 200710048312A CN 101229922 B CN101229922 B CN 101229922B
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Abstract
The invention relates to a method for extracting potassium from straws which adopts the water as leaching agent, uses microwave technique to damage fibrous tissue structure of the straws so that the potassium in the straws are precipitated in the form of ions; ion exchanger such as cation exchange resin or zeolite are used for separating and leaching the potassium in the solution; the solution such as hydrochloride, sulfate, nitric acid and so on are adopted to carry out the extrication; extrication liquid is evaporated, concentrated and crystallized to obtain the corresponding potassium salt products such as potassium chloride, potassium sulfate, potassium nitrate and so on. The experimental result displays that: extraction rate of the potassium in the straws can reach more than 70 percent and the concentration of the potassium in leaching solution can reach 3.6g/l. The method is also applied to the extraction of the potassium in the analog substances like wheat, corns, bamboos, trees and so on.
Description
Technical field:
The potash fertilizer of drawing from soil in the plant growing process, significant proportion exists in the stalk.And stalk wherein contains a large amount of potassium resources and is necessary to recycle as a kind of waste material of agriculture production.What the present invention relates to is recovery method to potassium in the wastes of crops stalk.The i.e. K in the stalk under microwave treatment
+Be dissolved in the leaching solution, potassium in spent ion exchange resin or the inorganic ion exchanger adsorbing and extracting liquid, select for use solution drip washing such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid to separate potassium on deresination or the ion-exchanger, evaporation concentration is freed liquid, and crystallization obtains various sylvite products.Present method both can be used for the extraction of potassium in straw, corn, the wheat stalk, can be used for the extraction of potassium in bamboo, the trees class material again, was used for paper industry simultaneously, reclaimed the potassium in the raw materials such as the used timber of papermaking, bamboo, stalk.
Background technology:
China is that large agricultural country is again the country of a potassium resource scarcity simultaneously, and nearly 5,000,000 tons of the required potassium product of annual industrial and agricultural production wherein 50% extracts from bittern, makes an appointment with half to need from external import.Meanwhile, after the potash fertilizer that is manured into soil was absorbed by crop, major part was enriched in the crop material, along with the harvestings of farm crop constantly is pulled away, cause soil potassium to wane gradually, the fertilising demand is increasing, has become one of important factor of restriction China agriculture production sustainable and stable development.
Agricultural crop straw is common agricultural wastes, has the characteristics wide, that stock number is big that distribute.The tool document announcement, potassium content reaches 1.89%, 1.18% and 1.94% respectively in rice straw, straw and the rape stalk, and sweet potato, potato stalk potassium content can reach more than 3%.The recovery and utilization technology of potassium mainly contains two kinds in the stalk at present, and a kind of is also field, burning back, though can solve the recovery problem of potassium resource, causes serious environmental to pollute simultaneously; Another kind is a direct returning to farmland, because the potassium speed of separating out makes that slowly wherein potassium can not be fine by plant absorbing in the stalk, simultaneously a large amount of straw directly returning to field brings detrimentally affect to soil.Document announcement is arranged with in the thermochemistry conversion of stalk as fuel, basic metal such as the potassium in the stalk, sodium are separated out pyrolysis, cause that heating surface is stained, a series of problems such as pollution and ash erosion, poly-group, prior separation and Extraction alkali metals such as potassium wherein, it also is favourable that the stalk thermochemistry is transformed.Yet, from stalk, extract the potassium technology and do not appear in the newspapers.
From the contextual analysis of organization of stalk as can be known, the crystallinity Mierocrystalline cellulose that forms between the complex construction that Mierocrystalline cellulose and xylogen constitute in the stalk and Mierocrystalline cellulose and the Mierocrystalline cellulose makes the destruction of stalk acquire a certain degree of difficulty.The key that stalk is put forward the potassium technology is to seek the method for effective processing stalk, to greatest extent contained potassium in the rational and effective dissolving stalk.Yet, in existing domestic and foreign literature, do not see relevant report as yet.
Summary of the invention:
At above-mentioned situation, the purpose of this invention is to provide and a kind ofly can carry out the method that effective molten lixiviate is got potassium in the stalk.This method both can be used for the extraction of potassium in straw, corn, the wheat stalk, can be used for the lixiviate of potassium in bamboo, the trees class material again.
The molten leaching of a kind of micro-wave digestion to potassium in the stalk goes out method, it is characterized in that: to the crushed straws water carry out molten soak processing after, with Zeo-karb or inorganic ion exchanger concentration and separation potassium wherein, and with containing NO
3 -Or SO
4 2-Aqueous solution drip washing free, free liquid and obtain KNO through evaporating, concentrating and crystallizing
3Or K
2SO
4Product; The time of described micro-wave digestion is 2-30 minute, and the solid-to-liquid ratio of stalk and water is 1: 20～1: 80, described to the crushed straws water carry out molten soak to handle be meant to crushed stalk to the 40-200 order water micro-wave digestion again.
For the structure quite stable stalk that constitutes by the crystallinity Mierocrystalline cellulose that forms between Mierocrystalline cellulose and xylogen and Mierocrystalline cellulose and the Mierocrystalline cellulose, except that can its structure deteriorate being obtained the corresponding inorganic metal ion, test shows, by certain leaching agent with the micro-wave digestion form, impel that potassium is dissolved in the leaching agent in the stalk, can reach and destroy its original weave construction, thereby sylvite required for the present invention is dissolved in the leaching solution and reaches the recovery purpose.Leaching agent can be water or contain mineral acid or the aqueous solution of salt, organic reagent.
So the present invention adopts the micro-wave digestion method that can destroy the stalk structure to make wherein, and potassium is dissolved in leaching agent and reaches the purpose of extracting potassium.
Can realize above-mentioned purpose of the present invention and a lot of as the inorganic salt of leaching agent or acid and/or organic compounds composition except that considering economic factors, serves as preferred to avoid or to reduce the compound that environment is polluted as far as possible also during selection.
The present invention investigated by experiment water, nitric acid, hydrochloric acid, perchloric acid, etc. solution to the solublization of stalk, the said leaching agent of the present invention, to above-mentioned for the multiple leaching agent composition selected for use, both can only adopt the composition form of single component, also can adopt two or more compositions to mix the form of forming, can decide according to concrete composition of stalk and situation.Test shows, it is different that different leaching agent compositions molten soaked on the effect performance.Water, nitric acid, hydrochloric acid, etc. some inorganic solutions the test of the solublization of the rice straw in eastern suburb, Chengdu is shown that the solubility rate of potassium all can reach more than 85%, and is wherein best with the solubilizing effect of water, nitric acid, reaches 89% and 92% respectively.Because nitric acid has oxidisability, can quicken the vegetable fibre oxidation dissolution in leaching agent, increase the later stage separating difficulty, and corrosive equipment is for water, except that having the good solubility energy, also having nontoxic, inexpensive, little to stalk post-processed influence characteristics, is good leaching agent.
By the experiment of further experiment chamber, micro-wave digestion stalk and ion exchange extraction potassium technological line and processing condition have been proposed, promptly be leaching agent with water, the micro-wave digestion stalk, Zeo-karb or inorganic ion exchanger extract potassium.
When adopting the molten method of soaking to extract stalk potassium, conditions such as temperature (T), the broken particle diameter of stalk, leaching agent amount, digestion time are all relevant with potassium dissolution rate in the stalk.Experiment shows that along with temperature raises, the growth of digestion time can increase the leaching velocity and the leaching yield of potassium in the stalk, but has also strengthened the fiber substance stripping in the stalk simultaneously, and this separates for follow-up potassium and brings difficulty.Optimal temperature is relevant with stalk composition and shelf-time with the time, and for clearing up of rice straw, suiting to clear up condition is that temperature is controlled at 40～80 ℃, and the time was at 2-10 minute.Be appreciated that the crushed stalk particle diameter is bigger to potassium stripping influence, along with the broken particle diameter of stalk reduces, dissolution rate and dissolution rate all improve.The leaching agent amount generally is controlled between the solid-to-liquid ratio 1: 20 to 1: 80, wherein with 1: 25 best results.The leaching agent amount is low excessively, and the potassium leaching yield reduces, and fiber substance concentration is bigger in the leach liquor that obtains, and causes liquid phase viscosity excessive, and is unfavorable to follow-up ion-exchange fractionation by adsorption; The leaching agent amount is too much, has increased ion-exchange absorption treatment capacity.Experiment shows that solution leaching method of the present invention is in above-mentioned condition and range, and the leaching yield of potassium reaches more than 90% in the stalk, and extracting solution is K in the sylvite product that resin isolation enrichment post crystallization obtains
2O content reaches more than 45%.
Description of drawings:
Figure of description is the process flow sheet that extracts potassium in the stalk with microwave method.Extracting solution makes the potassium product through exchange fractionation by adsorption, condensing crystal, separation.Liquid phase 2 bases wherein potassium concn height can turn back to drip washing operation and condensing crystal operation respectively.
Embodiment:
Example 1
This example is a raw material with eastern suburb, Chengdu stalk, and K content is 3.2% in the stalk.Get stalk 100g, be crushed to 200 orders, adding distil water 2500ml micro-wave digestion, digestion time 3 minutes, potassium leaching yield 90.6% in the digestion solution.Extracting solution through Zeo-karb enrichment, evaporation concentration, to obtain sylvite purity be 45.3% (K
2O).
Example 2
This example is a raw material with western suburb, Chengdu stalk, and K content is 2.8% in the stalk.Get stalk 200g, be crushed to 120 orders, adding distil water 5000ml micro-wave digestion, digestion time 3 minutes, potassium content 89.3% in the digestion solution.Extracting solution through Zeo-karb enrichment, evaporation concentration, to obtain sylvite purity be 45.1% (K
2O).
Claims (1)
1. the molten leaching of the micro-wave digestion to potassium in the stalk goes out method, it is characterized in that: to the crushed straws water carry out molten soak processing after, with Zeo-karb or inorganic ion exchanger concentration and separation potassium wherein, and with containing NO
3 -Or SO
4 2-Aqueous solution drip washing free, free liquid and obtain KNO through evaporating, concentrating and crystallizing
3Or K
2SO
4Product; The time of described micro-wave digestion is 2-30 minute, and the solid-to-liquid ratio of stalk and water is 1: 20～1: 80, described to the crushed straws water carry out molten soak to handle be meant to crushed stalk to the 40-200 order water micro-wave digestion again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710048312XA CN101229922B (en) | 2007-01-23 | 2007-01-23 | Method for abstracting potassium from straw by microwave technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710048312XA CN101229922B (en) | 2007-01-23 | 2007-01-23 | Method for abstracting potassium from straw by microwave technique |
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| Publication Number | Publication Date |
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| CN101229922A CN101229922A (en) | 2008-07-30 |
| CN101229922B true CN101229922B (en) | 2010-08-25 |
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|---|---|---|---|
| CN200710048312XA Expired - Fee Related CN101229922B (en) | 2007-01-23 | 2007-01-23 | Method for abstracting potassium from straw by microwave technique |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016788A (en) * | 2015-04-24 | 2015-11-04 | 南通蛇类治疗研究所 | Technological method for extracting potash fertilizers from straws |
| CN105601945A (en) * | 2016-02-01 | 2016-05-25 | 上海应用技术学院 | Method for preparing bio-based polyether polyol by carrying out microwave-assisted liquefaction on rape stalks |
| CN110754665A (en) * | 2019-10-30 | 2020-02-07 | 南宁学院 | Method for extracting potassium element from beef tripe |
| CN113135580B (en) * | 2021-06-01 | 2023-03-17 | 吉林海资生物工程技术有限公司 | Process for preparing artificial carnallite and potassium chloride by extracting potassium from corn soaking solution |
| CN113135581B (en) * | 2021-06-01 | 2023-01-24 | 吉林海资生物工程技术有限公司 | Process for preparing magnesium potassium sulfate and potassium sulfate by extracting potassium from corn soaking liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020143175A1 (en) * | 2001-03-27 | 2002-10-03 | Council Of Scientific & Industrial Research | Process for synthesis of a porphyrin compound using a molecular sieve catalyst under microwave irradiation |
| CN1792797A (en) * | 2005-12-28 | 2006-06-28 | 河北工业大学 | Process for preparing potassium sulfate by sea water |
-
2007
- 2007-01-23 CN CN200710048312XA patent/CN101229922B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020143175A1 (en) * | 2001-03-27 | 2002-10-03 | Council Of Scientific & Industrial Research | Process for synthesis of a porphyrin compound using a molecular sieve catalyst under microwave irradiation |
| CN1792797A (en) * | 2005-12-28 | 2006-06-28 | 河北工业大学 | Process for preparing potassium sulfate by sea water |
Non-Patent Citations (4)
| Title |
|---|
| 张胜帮等.微波消解电感耦合等离子体发射光谱法测定葛根中钾元素的研究.温州师范学院学报（自然科学版）22 6.2001,22(6),38-40. |
| 张胜帮等.微波消解电感耦合等离子体发射光谱法测定葛根中钾元素的研究.温州师范学院学报(自然科学版)22 6.2001,22(6),38-40. * |
| 程明芳等.应用离子交换树脂膜测定土壤钾素有效性的研究.土壤肥料 2.2000,(2),41-43. |
| 程明芳等.应用离子交换树脂膜测定土壤钾素有效性的研究.土壤肥料 2.2000,(2),41-43. * |
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|---|---|
| CN101229922A (en) | 2008-07-30 |
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