CN109081924A - A kind of feeding sodium humate and its preparation method and application - Google Patents

A kind of feeding sodium humate and its preparation method and application Download PDF

Info

Publication number
CN109081924A
CN109081924A CN201811239594.6A CN201811239594A CN109081924A CN 109081924 A CN109081924 A CN 109081924A CN 201811239594 A CN201811239594 A CN 201811239594A CN 109081924 A CN109081924 A CN 109081924A
Authority
CN
China
Prior art keywords
sodium
flocculation reaction
preparation
flocculant
flocculation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811239594.6A
Other languages
Chinese (zh)
Inventor
白义
刘建伟
张旭昊
白婷
付梦璐
张永飞
杨雅丽
殷春平
陈向阳
王凯
樊洁
马钰莹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningxia Xinyuan Biotechnology Co Ltd
Original Assignee
Ningxia Xinyuan Biotechnology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningxia Xinyuan Biotechnology Co Ltd filed Critical Ningxia Xinyuan Biotechnology Co Ltd
Priority to CN201811239594.6A priority Critical patent/CN109081924A/en
Publication of CN109081924A publication Critical patent/CN109081924A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08HDERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances

Landscapes

  • Chemical & Material Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Zoology (AREA)
  • Animal Husbandry (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

The present invention provides a kind of feeding sodium humates and its preparation method and application, belong to animal feed preparation field.The present invention is using lignite or weathered coal as raw material, and using sodium hydroxide as extractant, the preparation of sodium humate is realized using chemical synthesis process, addition chelating precipitation agent and two step flocculences.In the present invention, black, ulmic acid and fulvic acid are extracted with extractant sodium hydroxide first;Chelating precipitation agent is added, makes the separation of metal ions in conjunction with humic acid, settle, reduce the content of heavy metal and divalent oxonium ion in product, and deposition efficiency is high, and the yield of sodium humate is made to improve 5~10%;Flocculant is added, the colloidal sol electricity multimeric state of solution can be broken, insoluble matter is made to reunite, increase the volume and weight of insoluble matter, accelerate its sedimentation, to remove a large amount of insoluble matter in product;Final product purity obtained is high, insolubles content is few, heavy metal is few, as the application of feed addictive suitable for animal-breeding.

Description

A kind of feeding sodium humate and its preparation method and application
Technical field
The present invention relates to field of fodder, in particular to a kind of feeding sodium humate and its preparation method and application.
Background technique
Feeding sodium humate is the solid sheet object of brownish black slightly metallic luster, soluble easily in water, is in sepia after molten water Or dark solution, be in alkalescent, contain phenolic hydroxyl group, hydroxyl, carboxyl, quinonyl, carbonyl isoreactivity functional group, have absorption, be complexed, The functions such as ion exchange are mainly used as in animal sterilization, antibacterial, promote digestion, heavy metal etc. of degrading.
Currently, the purifying of sodium humate will lean on sulfuric acid or nitric acid acidwashing to remove the heavy metal in product substantially, in life There is a large amount of waste liquid during producing and discard, there is very big harm to environment and soil;In addition, what is retained in the product is a large amount of Sulfate radical and nitrate anion are also unfavorable for using in the product.Also, contain a large amount of silicate and heavy metal in its water-insoluble, Limit application of the sodium humate in field of fodder.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of feeding sodium humates and its preparation method and application.This hair It is bright to use chelating precipitation agent method and two step flocculences, keep the sodium humate being prepared with high purity, water-insoluble and heavy metal contain It measures low, is conducive in the industries such as animal husbandry as feed.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
The present invention provides a kind of preparation methods of feeding sodium humate, comprising the following steps:
1) after mixing the powder of feed coal, water, sodium hydroxide with chelating precipitation agent, reaction is extracted, is extracted Reaction solution, the feed coal are weathered coal or lignite;
2) the extraction reaction solution is mixed with the first flocculant, carries out the first flocculation reaction, obtains the first flocculation reaction Supernatant;
3) the first flocculation reaction supernatant is mixed with the second flocculant, carries out the second flocculation reaction, obtains second Flocculation reaction liquid;
4) the second flocculation reaction liquid is dry, obtain sodium humate.
Preferably, the powder of the feed coal, water, sodium hydroxide and the mass ratio of chelating precipitation agent be 1:5~8:0.1~ 0.2:0.04~0.06.
Preferably, the temperature that reaction is extracted in the step 1) is 70~90 DEG C, and the time is 1~3h.
Preferably, chelating precipitation agent is sodium citrate, disodium ethylene diamine tetraacetate, sodium pyrophosphate, phosphorus in the step 1) One or more of sour trisodium and polyphosphate sodium.
Preferably, in the step 2) the first flocculant and the second flocculant independently be sodium bicarbonate, potassium hydrogen phosphate and One or both of acrylamide.
Preferably, the dosage of the first flocculant is extract reaction solution volume 0.002~0.008% in the step 2).
Preferably, in the step 3) the second flocculant dosage be the first flocculation reaction supernatant volume 0.001~ 0.004%.
Preferably, the time of the first flocculation reaction is 2~3h, the second flocculation reaction in the step 3) in the step 2) Time be 1~2h.
The present invention also provides sodium humate made from preparation method described in above-mentioned technical proposal, the sodium humate is piece Shape, for water-insoluble less than 1%, content of beary metal is not higher than 8.5ppm, and humic acid content is not less than 70%.
The conduct in animal-breeding the present invention also provides sodium humate made from preparation method described in above-mentioned technical proposal The application of feed.
The present invention provides a kind of preparation methods of feeding sodium humate, comprising the following steps: 1) by the powder of feed coal, After water, sodium hydroxide are mixed with chelating precipitation agent, reaction is extracted, obtains extracting reaction solution, the feed coal is weathered coal Or lignite;2) the extraction reaction solution is mixed with the first flocculant, carries out the first flocculation reaction, obtains the first flocculation reaction Liquid;3) the first flocculation reaction liquid is mixed with the second flocculant, carries out the second flocculation reaction, obtains the second flocculation reaction Liquid;4) the second flocculation reaction liquid is dry, obtain sodium humate.The present invention is using lignite or weathered coal as raw material, with hydrogen-oxygen Change sodium is extractant, and chelating precipitation agent method is added and two step flocculences realize the preparation of sodium humate.In the present invention, it uses first Sodium hydroxide extractant extracts humic acid, ulmic acid and fulvic acid;It, will be with humic acid knot again by chelating precipitation agent The separation of metal ions of conjunction, sedimentation significantly reduce the content of heavy metal and divalent oxonium ion in product, and deposition efficiency is high, makes The yield of sodium humate improves 5~10%;Flocculation reaction twice is carried out after extracting reaction, it is therefore an objective to break the molten of solution Glue electricity multimeric state, makes insoluble matter reunite, and increases the volume and weight of insoluble matter, accelerates its sedimentation, to remove big in product The insoluble matter of amount, final sodium humate obtained is with high purity, insolubles content is few, heavy metal is few, suitable for animal-breeding Application as feed.Embodiment statistics indicate that, less than 1%, heavy metal contains sodium humate water-insoluble produced by the present invention Amount is not higher than 8.5ppm, and humic acid content is not less than 70%.
Specific embodiment
The present invention provides a kind of preparation methods of feeding sodium humate, comprising the following steps:
1) it extracts and reacts after mixing the powder of feed coal, water, sodium hydroxide with chelating precipitation agent, obtain extracting anti- Liquid is answered, the feed coal is weathered coal or lignite;
2) the extraction reaction solution is mixed with the first flocculant and carries out the first flocculation reaction, obtained in the first flocculation reaction Clear liquid;
3) the first flocculation reaction supernatant is mixed with the second flocculant and carries out the second flocculation reaction, obtain the second wadding Solidifying reaction solution;
4) the second flocculation reaction liquid is dry, obtain sodium humate.
The present invention extracts after mixing the powder, water, sodium hydroxide of feed coal with chelating precipitation agent to react, and is mentioned It extracts reaction solution;In the present invention, the feed coal is weathered coal or lignite.
In the present invention, it is preferred to pulverize to the feed coal, the powder of feed coal is obtained after crossing 300 meshes End.
In the present invention, the powder of the feed coal, water, sodium hydroxide and the mass ratio of chelating precipitation agent are preferably 1:5 ~8:0.1~0.2:0.04~0.06.
In the present invention, the temperature for extracting reaction is preferably 70~90 DEG C, and more preferably 75~85 DEG C, the time is preferred For 1~3h, more preferably 2h.
In the present invention, the sodium hydroxide is as extractant, by feed coal black, ulmic acid and fulvic acid extract Out.
In the present invention, the chelating precipitation agent is preferably sodium citrate, disodium ethylene diamine tetraacetate, sodium pyrophosphate, phosphorus One or more of sour trisodium and polyphosphate sodium.In the present invention, the chelating precipitation agent is by the metal in conjunction with humic acid Ion isolation, sedimentation significantly reduce the content of heavy metal and divalent oxonium ion in product, and deposition efficiency is high, improves The yield of sodium humate.The present invention does not have special restriction to the source of the chelating precipitation agent, using those skilled in the art Commercial goods known to member.
The present invention does not have special want to the powder of the feed coal, water, sodium hydroxide and the mixed method of chelating precipitation agent It asks, is mixed using method well known to those skilled in the art.
It obtains after extracting reaction solution, it is anti-that the extraction reaction solution is mixed the first flocculation of progress by the present invention with the first flocculant It answers, obtains the first flocculation reaction liquid.
In the present invention, the dosage of first flocculant is preferably extract reaction solution volume 0.002~0.008%.
In the present invention, the mixing is preferably stirred.
In the present invention, the time of the stirring is preferably 20~30min.
First flocculation is preferably evacuated in settling tank by the present invention, is precipitated 2~4h, is obtained the first flocculation reaction supernatant Liquid.
In the present invention, it is preferred to which the first flocculation reaction supernatant is extracted into agitator tank, mixed with the second flocculant The second flocculation reaction is carried out, the second flocculation reaction liquid is obtained.
In the present invention, the dosage of second flocculant be preferably the first flocculation reaction supernatant volume 0.001~ 0.004%.
In the present invention, the mixed mode preferably stirs.
In the present invention, the time of the stirring is preferably 20~30min.
In the present invention, first flocculant and the second flocculant be independently preferably sodium bicarbonate, potassium hydrogen phosphate and One or both of acrylamide.In the present invention, first flocculant and the second flocculant can break the molten of solution Glue electricity multimeric state, makes insoluble matter reunite, and increases the volume and weight of insoluble matter, accelerates its sedimentation, to remove big in product The insoluble matter of amount.The present invention does not have special restriction to the source of first flocculant and the second flocculant, using this field Commercial goods known to technical staff.
After obtaining the second flocculation reaction liquid, the present invention is dry by the second flocculation reaction liquid, obtains sodium humate.
The second flocculation reaction liquid is preferably evacuated in drying machine liquid bath and is dried by the present invention, and drying mode is preferably Roller drying, drying time are preferably 5~10s.
The present invention also provides sodium humate made from preparation method described in above-mentioned technical proposal, the sodium humate is piece Shape, for water-insoluble less than 1%, content of beary metal is not higher than 8.5ppm, and humic acid content is not less than 70%.
The conduct in animal-breeding the present invention also provides sodium humate made from preparation method described in above-mentioned technical proposal The application of feed addition.
Feeding sodium humate provided by the invention and the preparation method and application thereof is carried out below with reference to embodiment detailed Illustrate, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
1) weathered coal is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydrogen-oxygen Change sodium to mix with sodium citrate 1:8:0.1:0.04 in mass ratio, the mixed liquor is heated to 90 DEG C and extracts reaction, is held Continuous reaction 2h, obtains extracting reaction solution;
2) the first flocculant sodium bicarbonate is added in extracting reaction solution, the ratio that sodium bicarbonate is added is to extract reaction solution The 0.002% of volume stirs 20min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 2h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant sodium bicarbonate is added again, sodium bicarbonate is added Ratio is the 0.001% of the first flocculation reaction supernatant volume, continues to stir 20min, precipitates 1h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 5s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.91%, lead ion content 8.5ppm, Humic acid content is 76%, pH 9.8.
Embodiment 2
1) lignite is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydroxide Sodium is mixed with disodium ethylene diamine tetraacetate 1:8:0.1:0.045 in mass ratio, and the mixed liquor is heated to 90 DEG C and is extracted Reaction, sustained response 2h obtain extracting reaction solution;
2) the first flocculant potassium hydrogen phosphate is added in extracting reaction solution, the ratio that potassium hydrogen phosphate is added is to extract reaction solution The 0.003% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 2h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant potassium hydrogen phosphate is added, the ratio of potassium hydrogen phosphate is added It is the 0.002% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitate 1.5h, obtain the second flocculation reaction supernatant Liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 8s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.58%, lead ion content 8.1ppm, Humic acid content is 74%, pH 9.6.
Embodiment 3
1) weathered coal is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydrogen-oxygen Change sodium to mix with sodium pyrophosphate 1:7:0.1:0.05 in mass ratio, the mixed liquor is heated to 80 DEG C and extracts reaction, is held Continuous reaction 2h, obtains extracting reaction solution;
2) the first flocculant acrylamide is added in extracting reaction solution, the ratio that acrylamide is added is to extract reaction solution The 0.003% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 3h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant acrylamide is added again, acrylamide is added Ratio is the 0.001% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1.5h, obtain the second flocculation reaction Supernatant.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 10s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.29%, lead ion content 7.3ppm, Humic acid content is 78%, pH 9.6.
Embodiment 4
1) lignite is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydroxide Sodium is mixed with tertiary sodium phosphate 1:8:0.1:0.06 in mass ratio, and the mixed liquor is heated to 80 DEG C and extracts reaction, is continued 2h is reacted, obtains extracting reaction solution;
2) the first flocculant sodium bicarbonate is added in extracting reaction solution, the ratio that sodium bicarbonate is added is to extract reaction solution The 0.003% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 3h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, adds the second flocculant potassium hydrogen phosphate, the second flocculant is added Ratio is the 0.002% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1.5h, obtain the second flocculation reaction Supernatant.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 6s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.51%, lead ion content 7.2ppm, Humic acid content is 76%, pH 9.6.
Embodiment 5
1) weathered coal is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydrogen-oxygen Change sodium to mix with polyphosphate sodium 1:8:0.1:0.05 in mass ratio, the mixed liquor is heated to 80 DEG C and extracts reaction, is held Continuous reaction 2h, obtains extracting reaction solution;
2) the first flocculant sodium bicarbonate is added in extracting reaction solution, the ratio that sodium bicarbonate is added is to extract reaction solution The 0.005% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 2h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, adds the second flocculant acrylamide, the ratio of acrylamide is added Example is the 0.003% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1.5h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 7s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.31%, lead ion content 7.2ppm, Humic acid content is 79%, pH 9.8.
Embodiment 6
1) lignite is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydroxide Sodium is mixed with sodium citrate 1:8:0.1:0.05 in mass ratio, and the mixed liquor is heated to 80 DEG C and extracts reaction, is continued 2h is reacted, obtains extracting reaction solution;
2) the first flocculant potassium hydrogen phosphate is added in extracting reaction solution, the ratio that potassium hydrogen phosphate is added is to extract reaction solution The 0.006% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 2h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, adds the second flocculant acrylamide, the ratio of acrylamide is added Example is the 0.002% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1.5h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 8s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.32%, lead ion content 7.5ppm, Humic acid content is 77%, pH 9.7.
Embodiment 7
1) weathered coal is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydrogen-oxygen Change sodium to mix with disodium ethylene diamine tetraacetate 1:8:0.1:0.04 in mass ratio, the mixed liquor is heated to 80 DEG C and is extracted Reaction, sustained response 2h obtain extracting reaction solution;
2) the first flocculant acrylamide is added in extracting reaction solution, the ratio that acrylamide is added is to extract reaction solution The 0.006% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 3h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant sodium bicarbonate is added, the ratio of sodium bicarbonate is added It is the 0.003% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitate 1.5h, obtain the second flocculation reaction supernatant Liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 9s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.55%, lead ion content 7.8ppm, Humic acid content is 76%, pH 9.6.
Embodiment 8
1) lignite is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydroxide Sodium is mixed with (mixture of sodium citrate and sodium pyrophosphate) 1:8:0.1:0.05 in mass ratio, and the mixed liquor is heated to 80 Reaction DEG C is extracted, sustained response 2h obtains extracting reaction solution;
2) the first flocculant potassium hydrogen phosphate is added in extracting reaction solution, the ratio that potassium hydrogen phosphate is added is to extract reaction solution The 0.007% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 2h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, adds the second flocculant sodium bicarbonate, the ratio of sodium bicarbonate is added Example is the 0.004% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1.5h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 6s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.42%, lead ion content 7.5ppm, Humic acid content is 76%, pH 9.8.
Embodiment 9
1) weathered coal is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydrogen-oxygen Change sodium to mix with (mixture of disodium ethylene diamine tetraacetate and tertiary sodium phosphate) 1:8:0.1:0.05 in mass ratio, by the mixing Liquid is heated to 80 DEG C and extracts reaction, and sustained response 2h obtains extracting reaction solution;
2) the first flocculant sodium bicarbonate is added in extracting reaction solution, the ratio that sodium bicarbonate is added is to extract reaction solution The 0.008% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 3h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant sodium bicarbonate is added again, sodium bicarbonate is added Ratio is the 0.003% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 7s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.35%, lead ion content 7.4ppm, Humic acid content is 78%, pH 9.8.
Embodiment 10
1) lignite is pulverized, crosses 300 meshes, obtains feed coal powder;By feed coal powder, water, hydroxide Sodium is mixed with (mixture of sodium pyrophosphate and polyphosphate sodium) 1:8:0.1:0.05 in mass ratio, and the mixed liquor is heated to 80 Reaction DEG C is extracted, sustained response 2h obtains extracting reaction solution;
2) the first flocculant acrylamide is added in extracting reaction solution, the ratio that acrylamide is added is to extract reaction solution The 0.003% of volume stirs 30min, obtains the first flocculation reaction liquid;
3) the first flocculation reaction liquid is evacuated in settling tank, precipitates 3h, obtains the first flocculation reaction supernatant;By institute It states the first flocculation reaction supernatant to continue to be extracted into agitator tank, the second flocculant acrylamide is added again, acrylamide is added Ratio is the 0.004% of the first flocculation reaction supernatant volume, continues to stir 30min, precipitates 1h, obtain in the second flocculation reaction Clear liquid.
4) the second flocculation reaction supernatant is evacuated in drying machine liquid bath, by roller drying 8s, humic acid is made Sodium product.
Through detecting, in sodium humate product obtained above, water-insoluble 0.33%, lead ion content 7.6ppm, Humic acid content is 77%, pH 9.6.
The application of embodiment product
County of Guangdong Province makees additive with sodium humate prepared by the application, at more than 1600 families of more than 1,000 a production teams, 6000 bull pigs are raised, 350-500 grams of general daily gain is high up to 1900 grams.
Boar factory of county of Yunnan Province is added respectively to the pig of 13 all ages and classes with sodium humate prepared by the application Agent is raised 15 days, 690~1340 grams of average daily gain.
Based on the sodium humate of the application preparation, compound livestock and poultry growth regulator is made;The mother that lays eggs identical to 404 ages in days Chicken is tested.It is divided into control group and test group.Test group adds 1g sodium humate additive daily, and as a result test group compares 24.5% is improved according to group laying rate.
Sodium humate prepared by certain animal husbandry and fishery office of city the application seeks the laying rate of chicken, the plasma composition of chicken and egg The influence formed point is studied.Experiment chick 1016 is selected, is divided into control group and test group, test group is pressed in feed Ratio addition 1.5 ‰ -2 ‰ (is calculated) by scale, sodium humate content 79%, the results showed that (1) test group ratio control in 80 days Increase weight 85.6g more the average every chicken of group, improves weight gain 7.6%, significant difference (P < 0.01);(2) the test group death rate compares control group Reduce by 7.6% (P < 0.05);(3) test group is shown in that egg and opening produces the date and than control group shifts to an earlier date 2~5 days, 9 monthly average laying rate examinations It is higher than control group by 7.1% (P < 0.01) to test group;(4) test group feed to egg ratio is 3.06:1, control group 3.49:1;(5) test group egg Weight, volume, egg white weight and protein concentration have conspicuousness raising than control group.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of feeding sodium humate, includes the following steps:
1) it extracts and reacts after mixing the powder of feed coal, water, sodium hydroxide with chelating precipitation agent, obtain extracting reaction Liquid, the feed coal are weathered coal or lignite;
2) the extraction reaction solution is mixed with the first flocculant, carries out the first flocculation reaction, obtains the first flocculation reaction supernatant Liquid;
3) the first flocculation reaction supernatant is mixed with the second flocculant, carries out the second flocculation reaction, obtains the second flocculation Reaction solution;
4) the second flocculation reaction liquid is dry, obtain sodium humate.
2. preparation method according to claim 1, which is characterized in that the powder of feed coal, water, hydrogen-oxygen in the step 1) The mass ratio for changing sodium and chelating precipitation agent is 1:5~8:0.1~0.2:0.04~0.06.
3. preparation method according to claim 1 or 2, which is characterized in that extracting the temperature reacted in the step 1) is 70~90 DEG C, the time is 1~3h.
4. preparation method according to claim 1 or 2, which is characterized in that chelating precipitation agent is lemon in the step 1) One or more of sour sodium, disodium ethylene diamine tetraacetate, sodium pyrophosphate, tertiary sodium phosphate and polyphosphate sodium.
5. preparation method according to claim 1, which is characterized in that the first flocculant and the second flocculation in the step 2) Agent independently is one or both of sodium bicarbonate, potassium hydrogen phosphate and acrylamide.
6. preparation method according to claim 1 or 5, which is characterized in that the dosage of the first flocculant in the step 2) The 0.002~0.008% of reaction solution volume is extracted to be described.
7. preparation method according to claim 1 or 5, which is characterized in that the dosage of the second flocculant in the step 3) It is the 0.001~0.004% of the first flocculation reaction supernatant volume.
8. preparation method according to claim 1, which is characterized in that the time of the first flocculation reaction is in the step 2) 2~3h, the time of the second flocculation reaction is 1~2h in the step 3).
9. the sodium humate that preparation method described in claim 1~8 any one is prepared, the sodium humate is sheet, For water-insoluble less than 1%, content of beary metal is not higher than 8.5ppm, and humic acid content is not less than 70%.
10. sodium humate as claimed in claim 9 is in animal-breeding as the application of feed addictive.
CN201811239594.6A 2018-10-23 2018-10-23 A kind of feeding sodium humate and its preparation method and application Pending CN109081924A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811239594.6A CN109081924A (en) 2018-10-23 2018-10-23 A kind of feeding sodium humate and its preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811239594.6A CN109081924A (en) 2018-10-23 2018-10-23 A kind of feeding sodium humate and its preparation method and application

Publications (1)

Publication Number Publication Date
CN109081924A true CN109081924A (en) 2018-12-25

Family

ID=64843847

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811239594.6A Pending CN109081924A (en) 2018-10-23 2018-10-23 A kind of feeding sodium humate and its preparation method and application

Country Status (1)

Country Link
CN (1) CN109081924A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109796056A (en) * 2019-03-07 2019-05-24 内蒙古艾顿腐植酸科技有限公司 A kind of dedicated sheet sodium humate of aquaculture and its preparation process
CN109811014A (en) * 2019-01-10 2019-05-28 北京博思汇科生物技术有限公司 A method of feed addictive sodium humate is produced using bioactivity zymotechnic
CN110037174A (en) * 2019-04-04 2019-07-23 陕西艾顿腐植酸科技集团有限公司 A kind of feed grade sodium humate and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010108A (en) * 2010-10-08 2011-04-13 聊城金太阳生物化工有限公司 Industrial sludge treatment method and method for preparing various fertilizers by using treated industrial sludge
CN102558573A (en) * 2011-12-06 2012-07-11 中南大学 Method for extracting high-purity humic acid from low-rank coal
CN103613141A (en) * 2013-12-12 2014-03-05 徐万铭 Method for co-production of feed manganese sulfate by using wastewater of crude indium production
CN106220255A (en) * 2016-08-08 2016-12-14 彭亮 A kind of preparation method of fulvo acid sodium
CN106242881A (en) * 2015-10-20 2016-12-21 左文 A kind of preparation method improving humic acids quality

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010108A (en) * 2010-10-08 2011-04-13 聊城金太阳生物化工有限公司 Industrial sludge treatment method and method for preparing various fertilizers by using treated industrial sludge
CN102558573A (en) * 2011-12-06 2012-07-11 中南大学 Method for extracting high-purity humic acid from low-rank coal
CN103613141A (en) * 2013-12-12 2014-03-05 徐万铭 Method for co-production of feed manganese sulfate by using wastewater of crude indium production
CN106242881A (en) * 2015-10-20 2016-12-21 左文 A kind of preparation method improving humic acids quality
CN106220255A (en) * 2016-08-08 2016-12-14 彭亮 A kind of preparation method of fulvo acid sodium

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109811014A (en) * 2019-01-10 2019-05-28 北京博思汇科生物技术有限公司 A method of feed addictive sodium humate is produced using bioactivity zymotechnic
CN109796056A (en) * 2019-03-07 2019-05-24 内蒙古艾顿腐植酸科技有限公司 A kind of dedicated sheet sodium humate of aquaculture and its preparation process
CN110037174A (en) * 2019-04-04 2019-07-23 陕西艾顿腐植酸科技集团有限公司 A kind of feed grade sodium humate and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109081924A (en) A kind of feeding sodium humate and its preparation method and application
CN103214281B (en) Method for performing chemical innocent treatment on erythromycin waste residues and using erythromycin waste residues for producing organic fertilizer
US3775132A (en) Precipitation of metal proteinates from brines by base-acid-base hydrolysis
CN109400910A (en) A kind of neutrality sodium humate and its preparation method and application
CN102390914B (en) Method for suppressing hydrogen sulfide release in organic waste anaerobic process
CN109020630B (en) struvite and extraction method thereof
CN104892395B (en) Preparation method of ammonia manganese citrate
CN104803793B (en) Biologically active polypeptide prepares hard water resistance Water soluble fertilizer containing humic acid and method and application
CN106243177B (en) The preparation method of sucrose calcium complex
CN108117054A (en) A kind of method for preparing potassium dihydrogen phosphate coproduction ammonium potassium dihydrogen phosphate
CN108033527A (en) Improver of water quality and preparation method thereof
CN102874784A (en) Method for recovering nitrogen and phosphor from sewage by precipitation using concentrated seawater generated by sea water desalination
CN106831461B (en) A kind of synthesis technology of four sodium of iminodisuccinic acid
RU2709737C1 (en) Biologically active organo-mineral complex and a method for production thereof
CN103951024A (en) Method for separating calcium and magnesium ions in sodium chloride wastewater
CN105294314B (en) A kind of chelating fertilizer and preparation method thereof
CN105621582B (en) A kind of method of the water-soluble heavy metal ion of mechanical force curing
CN103011991A (en) Synergistic agent and preparation method thereof
KR20130142444A (en) Ion activation composite contains mineral extract by nitric acid hydrolysys and making process thereof
CN105565910A (en) Preparation method of bioactive polypeptide calcium fertilizer
CN104496654A (en) Method for preparing and using low-heavy-metal-content chlorella cultivation raw material mother solution
CN106927791B (en) Method for preparing fertilizer water solution and slow-release groove by using excess sludge
CN104555974A (en) Method for preparing lithium iron phosphate and lithium iron pyrophosphate by taking mineral leaching tail liquor as iron source
CN102863086A (en) Activator for aquaculture and preparation method thereof
Lominski et al. Production of staphylocoagulase in a chemically defined medium

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20181225