CN101830734B - Method for preparing potash fertilizer by using molasses alcohol waste mash - Google Patents
Method for preparing potash fertilizer by using molasses alcohol waste mash Download PDFInfo
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- CN101830734B CN101830734B CN2010101280177A CN201010128017A CN101830734B CN 101830734 B CN101830734 B CN 101830734B CN 2010101280177 A CN2010101280177 A CN 2010101280177A CN 201010128017 A CN201010128017 A CN 201010128017A CN 101830734 B CN101830734 B CN 101830734B
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Abstract
The invention relates to a method for preparing potash fertilizer by using molasses alcohol waste mash. The method comprises the following steps of: absorbing the potassium ions in the waste mash by using modified natural zeolite as an adsorbent; eluting the potassium ions in an adsorbing column by using ammonium sulfate or ammonium nitrate thermal solution to regenerate the zeolite to obtain a potassium-rich solution containing ammonium sulfate and potassium sulphate or ammonium nitrate and potassium nitrate; carrying out ammonia evolution on the potassium-rich solution after cooling; carrying out solid-liquid separation, washing the obtained solid phase, and drying to obtain the finished product of potassium sulphate or potassium nitrate. The obtained liquid phase of mother liquor containing potassium can be used for preparing eluent for next circulation after ammonia distillation, and ammonia obtained by the ammonia distillation can be used for ammonia evolution for the next circulation. The method for preparing the potash fertilizer has simple process and remarkable economic benefit and is easy for realizing industrial production, and the raw materials of the zeolite, the eluent and ammonia can be easily obtained and recycled.
Description
Technical field:
The invention belongs to the light industry technical field, specifically is a kind of method of producing potash fertilizer with molasses alcohol waste mash.
Background technology:
Vitriolate of tartar and saltpetre are a kind of fine chlorideless potassic fertilizers, are widely used in multiple kinds of crops, can use separately also to be used with nitrogenous fertilizer, phosphate fertilizer, and is especially more meaningful to some cash crop of " avoiding chlorine ".The main method of large-scale industrial production vitriolate of tartar had Mannheim proeess, metathesis conversion method and method such as from seawater and salt lake, extracted present stage, and the working method of saltpetre has SODIUMNITRATE and Repone K double decomposition and salt of wormwood or liquor kalii caustici to absorb the absorption process of nitric acid tail gas.The method that from the useless mash of molasses-spirit production, prepares agricultural potassium sulfate or saltpetre still is not reported.
Summary of the invention:
The objective of the invention is to propose a kind of method of producing potash fertilizer with molasses alcohol waste mash; Present method is to analyse technologies such as separation through absorption, wash-out, ammonia in the useless mash from molasses-spirit production; Preparation agricultural potassium sulfate or saltpetre make a marked difference choosing of raw material with existing method; Carry the later useless mash of potassium the disadvantageous effect of animal laxative effective is eliminated, through pervaporation, concentrate, dryly later can process animal-feed, improved the utility value of useless mash; From molasses alcohol waste mash, extract the present situation that potash fertilizer can be alleviated the agricultural potash fertilizer wretched insufficiency of China to a certain extent, have good social benefit, economic benefit and ecological benefits.
The present invention realizes through following technical scheme:
Produce the method for potash fertilizer with molasses alcohol waste mash; This method is a raw material with molasses alcohol waste mash, ammonia, industry or agricultural ammonium sulfate or an ammonium nitrate, with the natural zeolite of remodeling as the selective adsorbent of potassium ion, with industry or agricultural ammonium sulfate or ammonium nitrate solution as eluent; Obtain containing the rich potassium liquid of vitriolate of tartar and ammonium sulfate or saltpetre and an ammonium nitrate; Again with rich potassium liquid cooling but, ammonia analyses, solid-liquid separation, washing, drying and obtain finished product vitriolate of tartar or saltpetre, the advantage of this method is that wash-out is accomplished in same process with regeneration, does not need to carry out separately regenerative process; Simplified technical process, its concrete steps are following:
The first step, ammonium type prepare zeolite
Get natural zeolite and sieve, get sieve top, after boiling with saturated sodium chloride solution through the washing back; Use water washing, after boiling with saturated ammonium sulfate or ammonium nitrate solution again, use water washing; Make ammonium type zeolite, this ammonium type zeolite is packed in the stainless steel ionic adsorption post, subsequent use;
Second step, the preparation of rich potassium liquid
With getting after the useless mash cooling deposition in the ion selectivity adsorption column that upper strata liquid feeds the natural zeolite that remodeling is housed; At 10～50 ℃ the potassium ion in the useless mash is adsorbed; Hot soln with ammonium sulfate or an ammonium nitrate after absorption is accomplished is incubated wash-out as eluent; Obtain containing the rich potassium liquid of ammonium sulfate and vitriolate of tartar or saltpetre and an ammonium nitrate, zeolite is able to regeneration simultaneously, and water ejected the elutriant in the post after wash-out was accomplished;
The 3rd step, preparation finished product vitriolate of tartar or saltpetre
With the rich potassium liquid cooling of gained but, feed ammonia wherein vitriolate of tartar or saltpetre are separated out, after the concentration of ammonia acquires a certain degree; Stop logical ammonia and carry out solid-liquid separation; Solid phase obtains finished product vitriolate of tartar or saltpetre after with a certain amount of water washing drying, liquid phase is ammonia still process at a certain temperature, and the ammonia that steams is used for the ammonia of next round and analyses workshop section; The eluent preparation that mother liquor after the ammonia still process and top water are used for the next round operation realizes recycle.
The present invention compared with prior art has following beneficial effect:
It is higher to the present invention is directed in the molasses alcohol waste mash potassium content; And because the existence of potassium ion is to the disadvantageous effect as animal-feed; Proposition utilizes the ion selectivity absorption method to extract the potassium ion in the useless mash, both can therefrom obtain fine potash fertilizer, opens up the new way of preparation potash fertilizer; Can eliminate the laxative effective of useless mash again, have comprehensive economic benefit as animal-feed.Quality of potassium sulfate reaches the standard of acceptable end product among the GB20406-2006 among the present invention, and the quality of saltpetre reaches the standard of acceptable end product among the GB/T20784-2006, all can satisfy the purpose that agricultural is used; Through after the remodeling of natural zeolite is handled, the K uptake of zeolite is reached more than the 30g/L (zeolite) among the present invention.Because the zeolite that uses in the ion exchange column of the present invention just was improved to ammonium type zeolite before the k adsorption ion; And the potassium ion that on to the ammonium type zeolite in the ion exchange column, adsorbs when carrying out wash-out employed eluent be the salt that contains ammonium ion; Therefore can realize that wash-out and regeneration accomplishes in same process, not need independent regenerative process.The method technology that the present invention produces potash fertilizer is simple, is easy to realize suitability for industrialized production, and the raw material of use, zeolite, eluent and ammonia all are easy to get, and reusable edible, remarkable in economical benefits.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
As represent among Fig. 1 that molasses alcohol waste mash is got a certain amount of upper strata liquid and fed through in the natural zeolite ionic adsorption post of retrofiting potassium ion being adsorbed with certain speed after the overcooling deposition.After absorbing process is accomplished, use top water that a circulation produces and the potassium mother liquor after the ammonia still process and ammonium sulfate or an ammonium nitrate and be mixed with eluent the potassium ion that is adsorbed on the adsorption column is carried out wash-out, make the selective adsorption post be able to regenerate simultaneously.The elutriant that obtains promptly is rich potassium liquid; Use in the circulation ammonia that obtains after the cooling and carry out ammonia and analyse, carry out solid-liquid separation after accomplishing, the solid that obtains uses water washing and drying to be finished product vitriolate of tartar or saltpetre; The liquid phase mother liquor is used for next circulation and prepares eluent after ammonia still process is handled.Specific embodiment is following:
The preparation of embodiment one vitriolate of tartar
1. the remodeling of zeolite is handled
Take by weighing 10000 restrained 20～30 mesh sieves natural zeolite; Boil processing after 2 hours through the washing back with saturated sodium chloride solution, use water washing, carry out the same processing of boiling with saturated ammoniumsulphate soln again; The ammonium type natural zeolite that obtains retrofiting; Zeolite is packed in the adsorption column of Φ 50 * 3000mm jacketed, and loading amount is about 4.5 liters, and is subsequent use.
2. prepare rich potassium liquid
In above-mentioned ionic adsorption post, feeding useless mash with the flow velocity of 1SV from bottom to top adsorbs for 14 liters; Adsorption temp is 20 ℃; After absorption is accomplished the useless mash in the adsorption column is all discharged by the lower end, potassium content before and after the absorption and absorption and wash-out index are seen data in the table one.Use the potassium mother liquor that produces after the circulation ammonia still process and top water and industrial sulphuric acid ammonium and be mixed with eluant, eluent; For the first time make water and industrial sulphuric acid ammonium be mixed with eluant, eluent during wash-out in the present embodiment, get into circulating process and just can use later the potassium mother liquor that produces after the circulation ammonia still process and top water and industrial sulphuric acid ammonium and prepare eluant, eluent; The molal quantity of ammonium ion is 1.4 times of k adsorption ion molal quantity in the ionic adsorption post in the adjustment eluant, eluent; The potassium ion that 90 ℃ eluant, eluent adsorbs in the wash-out ionic adsorption post with the flow velocity of 3SV from top to bottom; The consumption of eluant, eluent is 2000ml, and the wash-out column temperature keeps 90 ℃, when obtaining stopping wash-out behind the rich potassium liquid 2000ml; Add top water 500ml again and collect top water liquid 500ml, the preparation process of rich potassium liquid is accomplished.
Above-mentioned " SV " is the abbreviated form of " space " and " velocity " two first letters of word; The meaning is a space velocity; The multiple that promptly per hour is equivalent to post mesolite volume through the useless mash of exchange column; The volume that per hour is meant the useless mash through 4.5 liters of zeolites like the 2SV in the present embodiment is about 4.5 * 1 liters, promptly per hour through 4.5 liters of useless mash.
3. prepare the finished product vitriolate of tartar
After the rich potassium liquid of the 2000ml that obtains in the said process is cooled to 20 ℃; When the amount of feeding ammonia reaches 30% (W/W); Ammonia is analysed technology and is finished, and under 20 ℃ of conditions, carries out solid-liquid separation, separates to obtain vitriolate of tartar 322.3 grams; Obtain potassium mother liquor 1650ml; The solid sulphuric acid potassium that obtains use its weight 10% the water spray Cleaning for High Capacity, be that the spray Cleaning for High Capacity water consumption is 322.3 * 10%=32.2 gram, through obtaining 287.5 gram vitriolate of tartar finished products after 105 ℃ of dryings, quality product meets acceptable end product requirement among the GB20406-2006.The liquid phase potassium mother liquor that obtains stops ammonia distillation process when 100 ℃ of following ammonia still processs reach ammonia content less than 0.1% (W/W), obtain the mother liquor 1400ml after the ammonia still process, and the ammonia amount that steams is 420.7 grams.
Material balance table in the table one preparation vitriolate of tartar process
The preparation of embodiment dinitric acid potassium
1. the remodeling of zeolite is handled
Take by weighing 10000 restrained 30～40 mesh sieves natural zeolite; Boil processing after 2 hours through the washing back with saturated sodium chloride solution, use water washing, carry out the same processing of boiling with saturated ammonium nitrate solution again; The ammonium type natural zeolite that obtains retrofiting; Zeolite is packed in the stainless steel adsorption column of Φ 50 * 3000mm jacketed, and loading amount is about 4.5 liters, and is subsequent use.
2. prepare rich potassium liquid
In above-mentioned selective adsorption post, feeding useless mash with the flow velocity of 1.2SV from bottom to top adsorbs for 15 liters; Adsorption temp is 30 ℃; After absorption is accomplished the useless mash in the selective adsorption post is all discharged by the lower end, potassium content before and after the absorption and absorption and wash-out index are seen data in the table two.Use the potassium mother liquor that produces after the circulation ammonia still process and top water and industrial ammonium nitrate and be mixed with eluant, eluent; For the first time make water and industrial ammonium nitrate be mixed with eluant, eluent during wash-out in the present embodiment, get into circulating process and just can use later the potassium mother liquor that produces after the circulation ammonia still process and top water and industrial ammonium nitrate and prepare eluant, eluent; The molal quantity of ammonium ion is 1.5 times of k adsorption ion molal quantity in the selective absorption post in the adjustment eluant, eluent; The potassium ion that adsorbs in the flow velocity wash-out selective absorption from top to bottom post of 80 ℃ eluant, eluent with 3.5SV; The consumption of eluant, eluent is 2000ml, and the wash-out column temperature keeps 80 ℃, when obtaining stopping wash-out behind the rich potassium liquid 2000ml; Add top water 500ml again and collect top water liquid 500ml, the preparation process of rich potassium liquid is accomplished.
3. prepare finished product saltpetre
After the rich potassium liquid of the 2000ml that obtains in the said process was cooled to 30 ℃, when the amount that feeds ammonia reached 20% (W/W), ammonia was analysed technology and is finished; Under 20 ℃ of conditions, carry out solid-liquid separation; Separate obtaining saltpetre 393.9 grams, obtain potassium mother liquor 1520ml, the solid nitric acid potassium that obtains is with the water spray Cleaning for High Capacity of its weight 5%; Through obtaining 342.7 gram saltpetre finished products after 105 ℃ of dryings, quality product meets acceptable end product requirement among the GB/T20784-2006.The liquid phase potassium mother liquor that obtains stops ammonia distillation process when 100 ℃ of following ammonia still processs reach ammonia content less than 0.1% (W/W), obtain the mother liquor 1400ml after the ammonia still process, and the ammonia amount that steams is 363.2 grams.
Material balance table in the table two preparation saltpetre process
Claims (2)
1. method of producing potash fertilizer with molasses alcohol waste mash; It is characterized in that this method is raw material with the molasses alcohol waste mash; As the selective adsorbent of potassium ion, as eluent, obtain containing the rich potassium liquid of vitriolate of tartar and ammonium sulfate or saltpetre and an ammonium nitrate with the natural zeolite of remodeling with industry or agricultural ammonium sulfate or ammonium nitrate solution; Again with rich potassium liquid cooling but, ammonia analyses, solid-liquid separation, washing, drying and obtain finished product vitriolate of tartar or saltpetre, concrete steps are following:
The first step, ammonium type prepare zeolite
Get natural zeolite and cross 10～60 mesh sieves, get sieve top, after process washing back is boiled 1～3 hour with saturated sodium chloride solution; Use water washing; After boiling 1～3 hour with saturated ammonium sulfate or ammonium nitrate solution again, use water washing, make ammonium type zeolite; This ammonium type zeolite is packed in the stainless steel ion selectivity adsorption column of jacketed, subsequent use;
Second step, the preparation of rich potassium liquid
Molasses alcohol waste mash is cooled to normal temperature also gets upper strata liquid after the deposition; Be equipped with in the ion selectivity adsorption column of ammonium type zeolite with the flow velocity feeding of 0.5～6SV from bottom to top; Under 10～50 ℃, the potassium ion in the useless mash is adsorbed, absorption is all discharged the useless mash in the selective adsorption post after accomplishing by the lower end; Get ammonium sulfate or an ammonium nitrate eluent that is mixed with soluble in water then, the mole number of ammonium ion is 1～3 times of k adsorption ion mole number in the selective adsorption post in the adjustment eluent, and this eluent is heated to 40～90 ℃, obtains the eluent hot soln; The eluent hot soln is carried out wash-out to the potassium ion that adsorbs in the ion selectivity adsorption column from top to bottom; Logical hot water in chuck makes the temperature of ion selectivity adsorption column in elution process remain on 40～90 ℃, when obtaining stopping wash-out behind the rich potassium liquid simultaneously; Water ejected the elutriant in the post after wash-out was accomplished; And collect top water liquid, and the preparation process of rich potassium liquid is accomplished, and zeolite is able to regeneration simultaneously;
The 3rd step, preparation finished product vitriolate of tartar or saltpetre
After second step, the rich potassium liquid that obtains was cooled to 20～30 ℃; Feeding ammonia separates out wherein vitriolate of tartar or saltpetre; When the amount that feeds ammonia reaches 10～30% by weight proportion, stop logical ammonia, carry out solid-liquid separation at normal temperatures; The solid phase that obtains is with the water spray Cleaning for High Capacity of its weight 5～10% (weight percent), obtains finished product vitriolate of tartar or saltpetre after being heated to 105 ℃ of dryings then; Liquid phase ammonia still process under 80～90 ℃ of temperature; Stop ammonia distillation process when reaching ammonia content less than 0.1% (W/W); The ammonia that steams is used for the ammonia of next round and analyses workshop section, and the top water liquid that the mother liquor after the ammonia still process and second step collect is used to prepare the eluent of next round operation, realizes recycle.
2. according to claim 1ly produce the method for potash fertilizer, it is characterized in that step is following with molasses alcohol waste mash:
The first step, ammonium type prepare zeolite
Get natural zeolite and cross 20～30 mesh sieves, get sieve top, after process washing back is boiled 2 hours with saturated sodium chloride solution; Use water washing, boil 2 hours with saturated ammonium sulfate or ammonium nitrate solution again after, use water washing; Make ammonium type zeolite; This ammonium type zeolite is packed in the stainless steel ion selectivity adsorption column of Φ 40 * 1500mm jacketed, and loading amount is 1.5 liters, and is subsequent use;
Second step, the preparation of rich potassium liquid
With molasses alcohol waste mash through being cooled to normal temperature and the deposition after; Getting 14 goes up layer liquid and feeds in the ion exchange column that ammonium type zeolite is housed with the flow velocity of 1SV from bottom to top and adsorb; Adsorption temp is 20 ℃, and absorption is all discharged the useless mash in the exchange column after accomplishing by the lower end; Get ammonium sulfate or an ammonium nitrate then and be dissolved in the 2000 mL water and be mixed with eluent, the mole number of ammonium ion is 1.5 times of k adsorption ion mole number in the selective adsorption post in the adjustment eluent, and this eluent is heated to 90 ℃, obtains the eluent hot soln; The eluent hot soln is carried out wash-out to the potassium ion that adsorbs in the ion exchange column from top to bottom; In chuck, lead to hot water simultaneously; Make the temperature of ion exchange column in elution process remain on 90 ℃,, add top water 500 mL again and collect top water liquid 500 mL when obtaining stopping wash-out behind rich potassium liquid 2000 mL; The preparation process of rich potassium liquid is accomplished, and the zeolite in the exchange column is able to regeneration simultaneously;
The 3rd step, preparation finished product vitriolate of tartar or saltpetre
After the rich potassium liquid of 2000 mL that obtain in the said process is cooled to 20～30 ℃; The amount that feeds ammonia reaches by weight proportion at 25% o'clock, and ammonia is analysed technology and finished, and carries out solid-liquid separation at normal temperatures; Separate and obtain vitriolate of tartar 322.3 grams; Obtain potassium mother liquor 1650mL, the solid sulphuric acid potassium that obtains is with the water spray Cleaning for High Capacity of its weight 5～10% (weight percent), obtains 287.5 gram vitriolate of tartar finished products after being heated to 105 ℃ of dryings then; The liquid phase potassium mother liquor that obtains stops ammonia distillation process when 100 ℃ of following ammonia still processs reach ammonia content less than 0.1% (weight percent); Obtain the mother liquor 1400mL after the ammonia still process; Mother liquor after this ammonia still process and the top water liquid of collecting in second step are used for preparing the eluent in second step of next round circulation; The ammonia amount that steams is 420.7 grams, the ammonia that steams be used in the 3rd step of next round circulation ammonia analyse operation, realize recycle.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102807235B (en) * | 2012-08-24 | 2015-04-22 | 广西力源宝科技有限公司 | Method for producing potassium sulfate by utilizing combustion ash content of molasses alcohol concentrated waste liquid |
| CN103253686B (en) * | 2013-05-03 | 2015-10-28 | 广东弘顺达环保生物科技投资有限公司 | A kind of method utilizing alcohol biological wastewater production vegetalitas xanthohumic acid/potassium sulfate concentrated solution/vegetalitas organic fungi-manure |
| CN103864472B (en) * | 2014-02-26 | 2016-03-09 | 化工部长沙设计研究院 | A kind of absorption method prepares the technique of potash fertilizer by potassium feldspar decomposition mother liquor |
| CN104030735A (en) * | 2014-07-07 | 2014-09-10 | 云南省轻工业科学研究院 | Preparation method of high-concentration water-soluble plant potash fertilizer |
| BR112018004742B1 (en) | 2015-09-10 | 2023-03-14 | Council Of Scientific & Industrial Research | PROCESS FOR POTASSIUM RECOVERY FROM BIOMETHANED WASHING WATER (BMSW) WITH CONCOMITANT IMPROVEMENT OF PROCESS EFFLUENT QUALITY |
| CN106068859A (en) * | 2016-06-30 | 2016-11-09 | 云南省农业科学院甘蔗研究所 | Liquid potash fertilizer application process in Caulis Sacchari sinensis field cultivation |
| CN106242685A (en) * | 2016-08-10 | 2016-12-21 | 云南省轻工业科学研究院 | Utilize the method that waste dreggy alcohol of sugar refinery and filter mud produce sugarcane special-purpose fertilizer |
| CN106220285A (en) * | 2016-08-10 | 2016-12-14 | 云南省轻工业科学研究院 | The method producing Liquid Fertilizer from alcohol waste mash |
| CN111328921A (en) * | 2020-03-11 | 2020-06-26 | 沈阳化工研究院有限公司 | Ruminant fermented feed and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1480430A (en) * | 2002-09-04 | 2004-03-10 | 莫志鸿 | Liquid fertilizer made from waste fluid of molasses and alcohol as well as its preparing method |
| CN101462899A (en) * | 2008-11-14 | 2009-06-24 | 林晓山 | Technique for producing humic acid organic compound fertilizer from sugar refinery waste slag and wastewater |
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| JPS6236094A (en) * | 1985-04-22 | 1987-02-17 | ト−ア化成株式会社 | Bad smell reducing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1480430A (en) * | 2002-09-04 | 2004-03-10 | 莫志鸿 | Liquid fertilizer made from waste fluid of molasses and alcohol as well as its preparing method |
| CN101462899A (en) * | 2008-11-14 | 2009-06-24 | 林晓山 | Technique for producing humic acid organic compound fertilizer from sugar refinery waste slag and wastewater |
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