CN104003425B - A kind ofly produce the novel process of sal enixum and the application in S-based compound fertilizer thereof - Google Patents

A kind ofly produce the novel process of sal enixum and the application in S-based compound fertilizer thereof Download PDF

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CN104003425B
CN104003425B CN201410251853.2A CN201410251853A CN104003425B CN 104003425 B CN104003425 B CN 104003425B CN 201410251853 A CN201410251853 A CN 201410251853A CN 104003425 B CN104003425 B CN 104003425B
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fertilizer
liquid
repone
nitration mixture
based compound
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CN104003425A (en
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刘天福
李秉政
张文星
刘卫平
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Hongri Chemical Co., Ltd., Shandong Prov.
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Shandong Hongri Acron Chemical Joint Stock Co Ltd
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Abstract

The invention belongs to technical field of agricultural fertilizers, disclose a kind of novel process of producing sal enixum, this technique employs lower-cost domestic white potassium, and the product chloride ion content of preparation is lower.The invention also discloses a kind of preparation technology of S-based compound fertilizer.Composite fertilizer prepared by the present invention effectively make use of agricultural waste material, and employs microbial fermentation technology, and holding water and fixing nitrogen effect is better, fertilizer efficiency is more lasting, rate of fertilizer reduces greatly, and energy-conserving and environment-protective simultaneously, achieve and turn waste into wealth.

Description

A kind ofly produce the novel process of sal enixum and the application in S-based compound fertilizer thereof
Technical field
The invention belongs to field of fertilizer production, be specifically related to a kind ofly produce the novel process of sal enixum and the application in S-based compound fertilizer thereof.
Background technology
" country's 12 planning outlines " are all classified as the series of problems such as grain security, Ecological Civilization Construction, energy-saving and emission-reduction in planning, and fertilizer plays a part very important as " grain in grain " in the enforcement of this planning.Within 2011, No.1 Central File more pays attention to water saving, in water saving, improves in utilization rate of fertilizer, is applicable to drip irrigation and spray irrigation fertilizer and more accords with the demands of the market.Market Water soluble fertilizer mostly is physics blending method secondary processing, relative waste of manpower, material resources, and mixes uneven, and fertilizer efficiency is unstable.
The development of China's fertilizer and application history, be main phase from farm manure to use inorganic fertilizer, because farm manure source of pollution are many, traffic capacity is large, operationally wastes time and energy and effect is not obvious especially; And inorganic fertilizer composition is single, utilization ratio is lower, and often causes soil compaction and adjoint soil erosion polluted source, influence ecological environment.The fertilizer of agricultural use mainly contains (NH in the early time 2) 2cO, (NH 4) 2sO 4, NH 4hCO 3, NH 4cl, (NH 4) 2hPO 4, NH 4h 2pO 4, NH 4nO 3the inorganic composite fertilizer etc. of calcium superphosphate, nitrophosphate fertilizer and Nitrogen-and Phosphorus-containing potassium.For the crop that vegetative period is longer, manuring late is also crucial.Except base fertilizer, topdress and generally all adopt NH 4hCO 3, NH 4cl, (NH 2) 2cO, NH 4nO 3deng, these all belong to mineral manure, and NH 4hCO 3, NH 4cl, (NH 4) 2sO 4, NH 4nO 3belong to ammonium fertilizer category Deng all, directly can be absorbed by crop, but because its volatilization is fast, utilization ratio is low, plant absorption is received and affects the drawbacks such as environment, not only increases production cost, and very easily cause water resource environment to worsen.(NH 2) 2cO belongs to acyl ammonium fertilizer, contained nitrogen need after the urine enzyme decomposition and inversion of urea bacterium secretion be ammonium nitrogen, can be absorbed by plants, its utilization ratio is generally 30 ~ 40%, and it has, and fertilizer efficiency utilization ratio is low, volatile, contaminate environment, precipitation, burning seedling burn the drawback such as leaf and soil compaction.In recent years, occurred some Chemical Mixed Fertilizers and biological organic fertilizer, which raises grain yield, and the fertilizer efficiency time length improves, and reduces the destructive force of environment; Such as Chinese patent CN102503650 discloses a kind of amino acid chelate fertilizer, this chelating fertilizer is by adding chelating amino acid and trace element, improve fertilizer efficiency, but it is higher to there is raw materials cost in this technology, need to add various trace elements and amino acid, general enterprises cannot bear high cost, and causing can not large-scale industrial production.
The sal enixum intermediate raw material that domestic production S-based compound fertilizer is used, mainly adopts the red Repone K of import and the vitriol oil to react in reactive tank.When building S-based compound fertilizer device before domestic 10 years, due to little to the demand of red potassium, import red potassium price and domestic white potassium difference less, and the advantage of red potassium is the low (W (H of moisture content 20) 0.2% one 0.5%), in pelletized form, K 2the high ((K of 0 content 20) 60% ~ 61%), steady quality, when reactive tank and sulfuric acid reaction, state is comparatively stable, and sal enixum overflow is also more stable, easy to operate, so domestic S-based compound fertilizer device uses the red potassium of import to produce S-based compound fertilizer always.Along with S-based compound fertilizer device gets more and more, the red potassium demand of import is increased fast.According to related statistical data, the red potassium of import per ton and domestic white potassium price difference are approximately about 100 yuan.In order to reduce costs, be necessary to produce S-based compound fertilizer with domestic white potassio for the red potassium of import.But use in domestic Repone K and there is following problem: 1,57% (K 20 content) Repone K moisture content is high, and in use slip surface flotation one deck material needs to be dissolved in water sometimes, and nitration mixture water content increases, cause compound fertilizer oven dry load large on the one hand, water content increases on the other hand, and hydrogenchloride is soluble in material oar, CI in material oar -content improves, CI in product -content also can correspondingly improve.Domestic Repone K moisture content is high, and viscosity is large, and conveying difficulty is large, and feed intake instability, causes compound fertilizer final product quality unstable.Use procedure overflow is unstable, causes finished product potassium content to fluctuate.2,60% (K 20 content) in use reactive tank emits vapour, nitration mixture density fluctuation is large, overflow is unstable, boiling explosion phenomenon etc.
Summary of the invention
The present invention be directed to the defect of prior art fertilizer production technology, a kind of novel process of producing sal enixum of proposition, this technique employs state's words spoken by an actor from offstage potassium, and cost reduces greatly, and chloride ion content is low.Present invention also offers a kind of S-based compound fertilizer and preparation technology thereof, this composite fertilizer effectively utilizes agricultural waste material, and employs microbial fermentation technology, and holding water and fixing nitrogen effect is better, fertilizer efficiency is more lasting, rate of fertilizer reduces greatly, energy-conserving and environment-protective simultaneously, achieve and turn waste into wealth.
For achieving the above object, the present invention is by the following technical solutions:
Produce a novel process for sal enixum, it comprises the steps:
Repone K raw material synchronously joins in reactor with worm conveyor and 98% vitriol oil after metering; The mol ratio of 98% vitriol oil and Repone K is 1.1:1; While reinforced, in reactor, pass into steam, the pressure 0.6Mpa of steam, vapor temperature 105 DEG C; In reactor, add Repone K and sulfuric acid continuously, do not stop to stir, mix and react, the hydrogen chloride gas generated in reaction process is extracted out by exhaust fan and is sent to absorption by Hydrochloric Acid operation, and it is for subsequent use that potassium hydrogen sulfate solution flow to nitration mixture groove.
Present invention also offers a kind of preparation technology of S-based compound fertilizer, it comprises the steps:
Repone K raw material synchronously joins in reactor with worm conveyor and 98% vitriol oil after metering, and wherein, the mol ratio of 98% vitriol oil and Repone K is 1.1:1; While reinforced, in reactor, pass into steam, the pressure 0.6Mpa of steam, vapor temperature 105 DEG C; Repone K and 98% vitriol oil is added continuously in reactor, do not stop to stir, mix while react, the hydrogen chloride gas generated in reaction process is extracted out by exhaust fan and is sent to absorption by Hydrochloric Acid operation, potassium hydrogen sulfate solution flow in nitration mixture groove and mixes with phosphoric acid, the two mass ratio is 2:3, stir through stirring rake and obtain nitration mixture, subsequently nitration mixture pump is driven in pelletizing drum, spray into liquefied ammonia simultaneously and carry out granulation and oven dry, be cooled to room temperature, then spray organic additive, stirrer stirs, cryodrying and get final product; Wherein, the mass ratio of nitration mixture, liquefied ammonia and organic additive is 10:3:1;
The preparation process of above-mentioned organic additive is as follows: dried by wheat stalk, then straw powder is ground into pulverizer, put in fermentor tank, in fermentor tank, add the water of dregs of beans, wheat bran and 100 DEG C subsequently, stir, during to be lowered to 30 DEG C, add composite bacteria liquid, under 100 revs/min of agitation conditions, ferment 48 hours, obtain fermented liquid; Wherein, the mass ratio of straw powder, dregs of beans, wheat bran, water and mixed bacteria liquid is 10:3:3:50:1; Described composite bacteria liquid is mixed by bacillus megaterium liquid, Bacillus licheniformis liquid, trichoderma harzianum liquid and the azotobacter chroococcum liquid volume ratio according to 1:1:1:1, and the concentration of four kinds of bacterium liquid is 1 × 10 8individual/ml.
Note, the bacterial classification used in above-mentioned steps is the conventional bacterial classification of this area, and those skilled in the art can obtain its bacterium liquid according to its conventional culture methods.Bacterial classification of the present invention all can be bought from commercial sources such as American Type Culture collection warehousings (ATCC) and obtain.
The beneficial effect that the present invention obtains mainly comprise following some:
Present invention process employs state's words spoken by an actor from offstage potassium, and cost reduces greatly, and the sal enixum chloride ion content of preparation is low.Composite fertilizer prepared by the present invention effectively make use of agricultural waste material, and employs microbial fermentation technology, and holding water and fixing nitrogen effect is better, fertilizer efficiency is more lasting, rate of fertilizer reduces greatly, greatly saves the cost of fertiliser production.The multiple-microorganism that the present invention selects adopts rational proportion, by symbiosis Relationship With Proliferation, defines a complexity and stable microecosystem, effectively fixed nitrogen fertilizer conservation, improves fertilizer efficiency; Preparation method of the present invention possesses the advantages such as flow process is short, energy consumption is low, environment friendly and pollution-free, is applicable to large-scale industrial production.
Embodiment
To the mode of specific embodiment be adopted to carry out detailed description to the present invention below, but should not be construed limitation of the present invention.
Embodiment 1
Produce a novel process for sal enixum, it comprises the steps:
Repone K raw material (domestic white potassium, weight in wet base number is at 1-2%) is transported in Repone K hopper, synchronously joins in reactor after metering with worm conveyor and 98% vitriol oil; The mol ratio of 98% vitriol oil and Repone K is 1.1:1.While reinforced, in reactor, pass into steam, to meet temperature requirement during conversion reaction, the pressure 0.6Mpa of steam, vapor temperature 105 DEG C, the continuous heating time is 5-10 minute.In reactor, add Repone K and sulfuric acid continuously, do not stop stir, mix and reacts, reach a certain amount of after flow out to back segment reactive tank from overflow port, in reactive tank continuation react generation potassium hydrogen sulfate solution.The hydrogen chloride gas generated in reaction process is extracted out by exhaust fan and is sent to absorption by Hydrochloric Acid operation, qualified potassium hydrogen sulfate solution flow in nitration mixture groove and mixes with phosphoric acid, the two mass ratio is 2:3, and stirring through stirring rake obtains meeting the nitration mixture of processing requirement, for workshop section of composite fertilizer.
Embodiment 2
A preparation technology for S-based compound fertilizer, it comprises the steps:
Repone K raw material (domestic white potassium, water content is at 1-2%) is transported in Repone K hopper, synchronously joins in reactor after metering with worm conveyor and sulfuric acid; The mol ratio of 98% vitriol oil and Repone K is 1.1:1.While reinforced, in reactor, pass into steam, to meet temperature requirement during conversion reaction, the pressure 0.6Mpa of steam, vapor temperature 105 DEG C, the continuous heating time is 5-10 minute.In reactor, add Repone K and sulfuric acid continuously, do not stop stir, mix and reacts, reach a certain amount of after flow out to back segment reactive tank from overflow port, in back segment reactive tank continuation react generation potassium hydrogen sulfate solution.The hydrogen chloride gas generated in reaction process is extracted out by exhaust fan and is sent to absorption by Hydrochloric Acid operation, qualified potassium hydrogen sulfate solution flow in nitration mixture groove and mixes with phosphoric acid, the two mass ratio is 2:3, stir through stirring rake and obtain meeting the nitration mixture of processing requirement, obtained nitration mixture pump is driven in pelletizing drum, sprays into liquefied ammonia simultaneously and carries out granulation and oven dry, then add organic additive, stirrer stirs, and to obtain final product; Wherein, the mass ratio of nitration mixture, liquefied ammonia and organic additive is 10:3:1.
The preparation process of organic additive is as follows: dried by wheat stalk, then straw powder is ground into pulverizer, put in fermentor tank, in fermentor tank, add the water of dregs of beans, wheat bran and 100 DEG C subsequently, stir, during to be lowered to 30 DEG C, add composite bacteria liquid, under 100 revs/min of agitation conditions, ferment 48 hours, obtain fermented liquid; Wherein, the mass ratio of straw powder, dregs of beans, wheat bran, water and mixed bacteria liquid is 10:3:3:50:1; Described composite bacteria liquid is mixed according to the volume ratio of 1:1:1:1 by bacillus megaterium liquid (ATCC15450), Bacillus licheniformis liquid (ATCC14580), trichoderma harzianum liquid (ATCC20873) and azotobacter chroococcum liquid (ATCC4412), and the concentration of four kinds of bacterium liquid is 1 × 10 8individual/ml.
Embodiment 3
The manure trial of composite fertilizer prepared by embodiment 2:
1. be test farm crop with wheat:
Control group: preparation method is with embodiment 2, and difference is not add organic additive;
Experimental group: fertilizer prepared by embodiment 2.
Experimental technique: be selected from blue Ling County economic and technological development zone experimental plot Winter Wheat Planted, the equal 10 mu of ground of experimental plot area that two groups of fertilizer processes respectively, control group usage quantity is 40kg/ mu, and experimental group is 30kg/ mu, and planting conditions is identical, possesses comparability.Gather in the crops wheat simultaneously, measure wheat per mu yield and stimulation ratio; Detect wheat grains per spike, thousand seed weight and per mu yield simultaneously.Specific experiment result: with reference to table 1.
Table 1
Group Grain number per spike Thousand seed weight (g) Per mu yield (kg)
Contrast 2 31.4 45.7 413
Experimental group 32.1 46.1 432
2. be test farm crop with paddy rice:
Control group: preparation method is with embodiment 2, and difference is not add organic additive;
Experimental group: fertilizer prepared by embodiment 2.
Experimental plot is positioned at test base, Mt. Mountain town, blue Ling County, rice cultivation, and the experimental plot area that four groups of fertilizer processes respectively is ten mu of ground, the usage quantity often organizing experimental plot fertilizer is 40kg, planting conditions is identical, gathers in the crops paddy rice simultaneously, measures paddy rice per mu yield and stimulation ratio; Detect paddy rice grain number per spike, thousand seed weight and unfilled gtains number simultaneously.
Experimental result: see table 2
Table 2
Group Unfilled gtains number (grain/fringe) Grain number per spike (grain/fringe) Thousand seed weight (g)
Control group 4.9 64.5 26.17
Experimental group 2.4 73.8 33.93
Found by wheat and Rice Cropping test, the fertilizer of experimental group is good, and the index such as grain number per spike and thousand seed weight is all better than control group, and can reduce the amount of application of fertilizer, reduces cost.
The specific embodiment of the present invention is described although above-mentioned in conjunction with the embodiments; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.

Claims (2)

1. a preparation technology for S-based compound fertilizer, it comprises the steps:
Repone K raw material synchronously joins in reactor with worm conveyor and 98% vitriol oil after metering, and wherein, the mol ratio of 98% vitriol oil and Repone K is 1.1:1; While reinforced, in reactor, pass into steam, the pressure 0.6MPa of steam, vapor temperature 105 DEG C; Repone K and 98% vitriol oil is added continuously in reactor, do not stop to stir, mix while react, the hydrogen chloride gas generated in reaction process is extracted out by exhaust fan and is sent to absorption by Hydrochloric Acid operation, potassium hydrogen sulfate solution flow in nitration mixture groove and mixes with phosphoric acid, the two mass ratio is 2:3, stir through stirring rake and obtain nitration mixture, subsequently nitration mixture pump is driven in pelletizing drum, spray into liquefied ammonia simultaneously and carry out granulation and oven dry, be cooled to room temperature, then spray organic additive, stirrer stirs, cryodrying and get final product; Wherein, the mass ratio of nitration mixture, liquefied ammonia and organic additive is 10:3:1;
The preparation process of described organic additive is as follows: dried by wheat stalk, then straw powder is ground into pulverizer, put in fermentor tank, in fermentor tank, add the water of dregs of beans, wheat bran and 100 DEG C subsequently, stir, during to be lowered to 30 DEG C, add composite bacteria liquid, under 100 revs/min of agitation conditions, ferment 48 hours, obtain fermented liquid; Wherein, the mass ratio of straw powder, dregs of beans, wheat bran, water and composite bacteria liquid is 10:3:3:50:1; Described composite bacteria liquid is mixed by bacillus megaterium liquid, Bacillus licheniformis liquid, trichoderma harzianum liquid and the azotobacter chroococcum liquid volume ratio according to 1:1:1:1, and the concentration of four kinds of bacterium liquid is 1 × 10 8individual/mL;
Described bacillus megaterium is ATCC15450, and described Bacillus licheniformis is ATCC14580, and described trichoderma harziarum is ATCC20873, and described azotobacter chroococcum is ATCC4412.
2. according to composite fertilizer prepared by technique described in claim 1.
CN201410251853.2A 2014-06-09 2014-06-09 A kind ofly produce the novel process of sal enixum and the application in S-based compound fertilizer thereof Active CN104003425B (en)

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CN105668593B (en) * 2015-12-30 2018-05-11 川恒生态科技有限公司 A kind of production method of acid sulphur potassium phosphate

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CN1272286C (en) * 2005-05-16 2006-08-30 西洋集团 Device for low-temperature continuous conversion of potassium chloride to heating steam and production process thereof
CN103044157B (en) * 2013-01-24 2014-05-07 山东红日阿康化工股份有限公司 Amino acid guniting compound fertilizer and preparation method thereof

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Address after: Luo Road 276021 Shandong city of Linyi province Luozhuang District No. 21

Patentee after: Hongri Chemical Co., Ltd., Shandong Prov.

Address before: Luo Road 276021 Shandong city of Linyi province Luozhuang District No. 21

Patentee before: Shandong Hongri Acron Chemical Joint Stock Co., Ltd.