CN103004872A - Method for preparing sanitizer and liquid potash fertilizer from cow dung as raw material - Google Patents

Method for preparing sanitizer and liquid potash fertilizer from cow dung as raw material Download PDF

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Publication number
CN103004872A
CN103004872A CN2013100143937A CN201310014393A CN103004872A CN 103004872 A CN103004872 A CN 103004872A CN 2013100143937 A CN2013100143937 A CN 2013100143937A CN 201310014393 A CN201310014393 A CN 201310014393A CN 103004872 A CN103004872 A CN 103004872A
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China
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cow dung
sulfuric acid
potash fertilizer
acid solution
raw material
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CN103004872B (en
Inventor
李霞
刘伟
刘小华
杜玲枝
张鸿云
申钰静
李盼盼
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Henan University of Urban Construction
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Henan University of Urban Construction
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
    • Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses

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Abstract

The invention discloses a method for preparing a sanitizer and a liquid potash fertilizer from cow dung as a raw material. The method is characterized by comprising the following steps of taking sulfuric acid solution in a three-necked flask, and adding 2-10 parts by weight of cow dung into 1000 parts by weight of sulfuric acid solution under a stirring condition, wherein the concentration of the sulfuric acid solution is 3-7mol/L; and heating a reaction system to 75-90 DEG C, adding 30-70 parts by weight of potassium chlorate after hydrolyzing, leading out generated ClO2 by a conduit, absorbing by water and/or alkaline aqueous solution to obtain the sanitizer, and preparing the liquid potash fertilizer from the residual mixture. The method disclosed by the invention is mild in reaction condition, high in reaction speed, complete in reaction, simple to operate, easy for raw material obtaining, and low in raw material cost; waste is fully changed into valuable resources; and a series of pollutions caused by the cow dung are solved. Therefore, the method has great significance on promotion of sustainable development of dairy cow and beef cattle breeding industry.

Description

The method for preparing disinfectant and liquid potash fertilizer take cow dung as raw material
Technical field
The invention belongs to the environmental protection agriculture field, relate in particular to the method for preparing high-pure chlorinedioxide and liquid potash fertilizer type compound fertilizer take cow dung as raw material.
Background technology
In the breeding process of ox, can produce a large amount of cow dungs, if do not utilize rationally and effectively, not only waste resource, simultaneously to causing of environment pollution (to the pollution of water, soil or atmosphere).Therefore effectively utilize the residue nutriment in the cow dung, realize recycling, the innoxious new direction that becomes research of discarded object.The composition that content is maximum in the cow dung is the crude fibre with reproducibility, and raw fiber is hydrolyzed the glucose that generates under acid condition can generate chlorine dioxide with the potassium chlorate reaction.Chlorine dioxide is a kind of good disinfectant, can be used for the purification of waste water in the vaccary, the realization water circuit utilizes, also can be used for disinfection of drinking water, food processing, vegetable and fruit are fresh-keeping, all many-sides such as water body disinfection of health and epidemic prevention sterilization and sterilization, aquaculture, contain the elements such as nitrogen phosphate and sulfur, iron, potassium, zinc in the reacted liquid, can be used as after treatment the fertilising that liquid fertilizer is used for the cattle farm grass.The preferably disinfection agent of chlorine dioxide of effect that can be sterilized again when eliminating discarded environmental pollution like this, resource is reasonably used.
At present processing and the utilization of cow dung are focused mostly in compost treatment, make animal and fowl fodder, life and the aspects such as generating biogas production and edible fungus culturing, but these application all have certain limitation.For example: in compost treatment, owing in the cow dung pathogen, worm's ovum, antibiotic etc. are arranged, and comparatively stable in compost treatment, in secondary utilizes, utilize improper be easy to cause water body and land pollution; Make in the animal and fowl fodder, because poor, the frowziness of palatability of cow dung ight soil, it is low and limited it and done the exploitation of feed to contain pathogen, parasite and digestibility, in addition, a large amount of various additives can remain in the ight soil in the breeding process of ox, when ight soil can be used as the feed use, the problem that additive exceeds standard even poisons may appear, so developed country has not advocated to use at present; In life and the generating biogas production, the cost of biogas engineering is generally higher, and investment is large, and operational effect is subjected to the impact in temperature, season large and limited the popularization that cow dung is just made biogas; In the edible fungus culturing, exist now and produce randomness greatly, the edible fungus quality is unstable, and the uppity shortcoming of production technology.
Summary of the invention
The object of the present invention is to provide and a kind ofly prepare high-purity disinfectant chlorine dioxide with cow dung as raw material; and be used for the method for aquaculture environmental protection and production safety protection; method by-product high concentration liquid potash fertilizer type compound fertilizer fertilizer can be used for agriculture circulation production and application in addition.The method, it is for achieving the above object, the present invention by the following technical solutions:
The present invention relates to a kind of method for preparing disinfectant and liquid potash fertilizer take cow dung as raw material, the sulfuric acid solution that it is characterized in that comprising the steps: to get is in three-neck flask, add in the sulfuric acid solution of 1000 weight portions the cow dung of situation about stirring with the 2-10 weight portion, the concentration of described sulfuric acid solution is 3-7mol/L, reaction system is heated to 75-90 degree centigrade, after the hydrolysis, add 30-70 weight portion potassium chlorate, will generate ClO with conduit 2Derivation, adopt water and/or alkaline aqueous solution to absorb the bactericide that is sterilized; Remaining mixture is for the preparation of liquid potash fertilizer, and the reaction time is more than 120 minutes, is preferably 140-180min.
In a preferred embodiment of the present invention, described remaining mixture filters, filtrate adds potassium hydroxide or potash modulation neutrality is prepared into liquid potash fertilizer, and this liquid fertilizer has made wherein in the ight soil remaining antibiotic, germ and other some organic matters and epidemic disease source microorganism clear up complete because using aborning high oxidation gonosome based environment.
In a preferred embodiment of the present invention, the ClO that derives 2Adopt 5 grades of absorptions, front level Four is frozen water, and level V is the sodium carbonate liquor of mass fraction 0.03-0.07%.
In another preferred embodiment of the present invention, described cow dung is dry cow dung.
The present invention also relates to a kind of integrated application method of cow dung on the other hand, and it comprises the above-mentioned method for preparing disinfectant and liquid potash fertilizer take cow dung as raw material, and prepared disinfectant is used for the sterilization in vaccary; Described liquid potash fertilizer is used for the grassland circulation and produces and/or agriculture grain-production.
Method of the present invention is in sulfuric acid medium, prepares high-pure chlorinedioxide with cow dung reductive hydrolysis sodium chlorate, and its reaction condition is gentle, and reaction is fast, and the product yield of institute is high, the purity height, and raw material is cheap and easy to get.There is the vaccary in China in the area greatly, select cow dung as reductant, its hydrolysis is used for the reduction preparation of chlorine dioxide from sodium chlorate, not only raw material is cheap and easy to get, effectively reduces production cost, has realized twice laid, a series of environmental pollutions that cow dung is brought have also been solved, and to developing distinctive agricultural undertakings and processing of agriculture product industry, prolong the agricultural production chain, it is significant to drive agricultural development.
Embodiment
Embodiment one:
Get the sulfuric acid solution of 100ml in three-neck flask, add the dry cow dung sample stirring and dissolving of 0.5001g in situation about stirring, reaction system is heated to 80 degrees centigrade, be hydrolyzed about 30 minutes, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), total reaction time is about 150min, till no longer producing to chlorine dioxide, with five content and the purity that go on foot the iodometric determination chlorine dioxide.Be converted into the chlorine dioxide percentage in chlorine in the potassium chlorate, chlorine dioxide productive rate 47.23%, purity is 98.60%.After residual solution is regulated the pH value with potassium hydroxide etc. after the reaction, obtain liquid potash fertilizer, with the content of tetraphenyl borate potassium gravimetric detemination potassium, with K 2O meter, percentage composition are greater than 30%, and its potassium content is high, use safety, and be better than directly using the cow dung fertilizer efficiency.
Embodiment two:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.6002g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L,, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 57.49%, purity are 97.04%.
Embodiment three:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.5001g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L,, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 63.15%, purity are 98.92%.
Embodiment four:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8006g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L,, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 66.01%, purity are 97.48%.
Embodiment five:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.9005g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L,, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 64.73%, purity are 97.86%.
Embodiment six:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 1.0012g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 62.66%, purity are 98.08%.
Embodiment seven:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8g in situation about stirring, reaction system is heated to 75 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 58.24%, purity are 98.48%.
Embodiment eight
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8g in situation about stirring, reaction system is heated to 80 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 63.85%, purity are 97.84%.
Embodiment nine:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8g in situation about stirring, reaction system is heated to 85 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 65.48%, purity are 98.08%.
Embodiment ten:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8g in situation about stirring, reaction system is heated to 90 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 64.60%, purity are 98.00%.
Embodiment 11:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 0.8g in situation about stirring, reaction system is heated to 85 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 4.5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 60.03%, purity are 97.08%.
Embodiment 12:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 1.0012g in situation about stirring, reaction system is heated to 85 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5.0moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 65.62%, purity are 98.32%.
Embodiment 13:
Get the sulfuric acid solution of 100ml in three-neck flask, add the cow dung sample stirring and dissolving of 1.0012g in situation about stirring, reaction system is heated to 85 degrees centigrade, after hydrolysis a period of time, add 5g potassium chlorate, the reaction system sulfuric acid concentration is 5.5moL/L, will generate ClO with conduit 2Derivation, adopt Pyatyi to absorb (front level Four is frozen water, and level V is the sodium carbonate liquor that mass fraction equals 0.05), the reaction time is about 150min, till no longer producing to chlorine dioxide, measures the content of chlorine dioxide with hypo solution.Chlorine dioxide productive rate 63.81%, purity are 97.79%.
Liquid and waste slag produced can with the sand core funnel filtration under diminished pressure to beaker, the adding potassium hydroxide or potash etc. and modulate neutrality, the treated liquid inorganic composite fertilizers that can be used as of mineral salt such as the potassium chloride that contains in the solution, potassium sulphate that produces during the invention process.
The present invention utilizes technology to compare following advantage with existing cow dung resource:
1. the present invention adopts cow dung in the sulfuric acid solution medium, and reduction potassium chlorate prepares high-purity disinfectant chlorine dioxide, and reaction condition is gentle, and reaction rate is fast, safe easy operating, and product purity is high.Both greatly reduce the high production cost of traditional chlorine dioxide electrolysis production and starch method chemical production, reduced again a series of environmental pollutions that cow dung is brought, and realized effective utilization of cow dung resource.
2. utilize chlorine dioxide to be used for the aquaculture wastewater treatment, have safety, low toxicity, characteristics that bactericidal effect is good, reduced present plant environment maintenance and safety and become to produce cost.
Residual night behind the preparation chlorine dioxide the treated liquid potash fertilizer type compound fertilizer fertilizer that gets, not only rationally utilize resource but also improved economic benefit, compare with traditional composting process, biogas method, this fertilizer has safety, other can cause the characteristics of secondary pollution material without epidemic disease source microorganism, antibiotic etc.
The above be the specific embodiment of the present invention only, but protection scope of the present invention is not limited to this, and any variation or replacement of expecting without creative work all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.

Claims (5)

1. method for preparing disinfectant and liquid potash fertilizer take cow dung as raw material, the sulfuric acid solution that it is characterized in that comprising the steps: to get is in three-neck flask, add in the sulfuric acid solution of 1000 weight portions the cow dung of situation about stirring with the 2-10 weight portion, the concentration of described sulfuric acid solution is 3-7mol/L, reaction system is heated to 75-90 degree centigrade, after the hydrolysis, add 30-70 weight portion potassium chlorate, will generate ClO with conduit 2Derivation, adopt water and/or alkaline aqueous solution to absorb the bactericide that is sterilized; Remaining mixture is for the preparation of liquid potash fertilizer, and the reaction time is more than 120 minutes, is preferably 140-180min.
2. method according to claim 1 is characterized in that described remaining mixture through filtering, and filtrate adds potassium hydroxide or potash modulation neutrality is prepared into liquid potash fertilizer.
3. method according to claim 1 is characterized in that the ClO that derives 2Adopt 5 grades of absorptions, front level Four is frozen water, and level V is the sodium carbonate liquor of mass fraction 0.03-0.07%.
4. the described method of any one according to claim 1-3, described cow dung is dry cow dung.
5. the integrated application method of a cow dung, it comprises the method for preparing disinfectant and liquid potash fertilizer take cow dung as raw material that claim 1-4 any one is described, prepared disinfectant is used for the sterilization in vaccary; Described liquid potash fertilizer is used for the grassland circulation and produces and/or agriculture grain-production.
CN201310014393.7A 2013-01-15 2013-01-15 Method for preparing sanitizer and liquid potash fertilizer from cow dung as raw material Expired - Fee Related CN103004872B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104777105A (en) * 2015-04-03 2015-07-15 四川省畜牧科学研究院 Detection technology for phosphorus in livestock and poultry excrement

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1230517A (en) * 1998-03-27 1999-10-06 黄君礼 Chlorine dioxide generating method and apparatus
CN101391750A (en) * 2008-10-30 2009-03-25 郑州大学 Method for preparing high-purity chlorine dioxide by using starchiness raw material and method for preparing catalyst used therein
CN101391751A (en) * 2008-10-30 2009-03-25 郑州大学 Method for preparing high-purity chlorine dioxide by using agronomic crop stalk and method for preparing catalyst used therein

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1230517A (en) * 1998-03-27 1999-10-06 黄君礼 Chlorine dioxide generating method and apparatus
CN101391750A (en) * 2008-10-30 2009-03-25 郑州大学 Method for preparing high-purity chlorine dioxide by using starchiness raw material and method for preparing catalyst used therein
CN101391751A (en) * 2008-10-30 2009-03-25 郑州大学 Method for preparing high-purity chlorine dioxide by using agronomic crop stalk and method for preparing catalyst used therein

Non-Patent Citations (1)

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Title
杜小旺等: "纤维素还原氯酸钠制备二氧化氯的研究", 《重庆师范大学学报（自然科学版）》, vol. 23, no. 3, 30 September 2006 (2006-09-30) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104777105A (en) * 2015-04-03 2015-07-15 四川省畜牧科学研究院 Detection technology for phosphorus in livestock and poultry excrement

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