CN105176536A - Preparation method of weathered coal humic acid water retention agent - Google Patents
Preparation method of weathered coal humic acid water retention agent Download PDFInfo
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Abstract
The invention discloses a preparation method of a weathered coal humic acid water retention agent, belonging to the technical field of agricultural drought resistance and water conservation. The preparation method comprises the following steps: immersing the raw material dried weathered coal in hydrochloric acid, washing with water, carrying out desalting treatment, carrying out soda boiling reaction, carrying out high-speed centrifugation to remove the precipitate to obtain humic acid, adding a dispersing agent and an organic solvent, and carrying out grafting reaction on an acrylic acid alkali solution and the humic acid by using potassium persulfate as an initiator, thereby obtaining the weathered coal humic acid water retention agent. The example proves that the method is simple to operate and easy to implement, is safe and sanitary, can be self-degraded without easily hardening the soil, improves the soil structure, and enhances the water/fertilizer utilization ratio of the crops by 85% or above.
Description
Technical field
The invention discloses a kind of preparation method of weathered coal humic acid water-holding agent, belong to coping with agriculture drought water conservation technical field.
Background technology
China be one vast in territory, resourceful large agricultural country.But natural disaster is serious, totally unfavorable to agricultural sustainable development, agriculture production is faced with stern challenge, and arid has become common a kind of natural disaster that people face, and current arid area accounts for world land area 40%, China is the country that a drought-hit area Area comparison is large, particularly northern 16 provinces and regions, cultivated area 5,200 ten thousand hectares, but mostly be typical semiarid zone, cause the waste of land resources, economical is inharmonious.
Because regional arid has had a strong impact on agricultural, production of forestry, water-loss reducer of soil is used to be to alleviate arid at present, improve the most frequently used method of efficiency of water application.Water-holding agent uses super absorbent resin, and it is the functional high molecule material that a kind of water-retaining capacity is strong especially, has water suction, water conservation, releases water function.It can rapidly specific absorption self tuple hundred doubly even thousand times deionized water, be expanded to hydrogel after wash water, can absorb for crop by slow releasing moisture, thus enhancing water retention, improvement Soil structure, reduces deep percolation and loss of soil nutrient, improves efficiency of water application.
In recent years, utilizing water-holding agent to improve Soil structure and improve crop liquid manure utilising efficiency, is the important way of chemical water-saving technology.At present, the kind of existing water conservation is a lot, has starch series, Mierocrystalline cellulose serial, the mixture of protein series and different classes of water-holding agent thereof.Wherein the starch graft copolymer water-holding agent water suction of producing and water retention high, but the problem such as it is poor to need solution to reduce costs with Saline alkali tolerance, and work-ing life is short.The reaction of synthesized polymer system water-holding agent is easy to realize and water-intake rate is higher, but is not easily biodegradable, and chemical agent easily causes soil compaction, and cost is higher.
Summary of the invention
The technical problem that the present invention mainly solves: more for current China arid area, have a strong impact on agricultural, forest development, although conventional water-loss reducer of soil can improve Soil structure, improve crop water and fertilizer utilization, but be by chemosynthesis mostly, not only cost compare is high, harvest volume is indirectly made to reduce, and chemical agent is more easily causes soil compaction, not easily be biodegradable, for the problem that environment is also a kind of invisible harm, provide a kind of preparation method of weathered coal humic acid water-holding agent, the method is for raw material with dry weathered coal, first use salt acid soak, desalting treatment after washing, react through soda boiling again, throw out is removed after high speed centrifugation, obtain humic acids, add dispersion agent and organic solvent afterwards, again with vinylformic acid alkaline solution for raw material, adding Potassium Persulphate is that initiator and humic acids carry out graft reaction and obtain a kind of weathered coal humic acid water-holding agent.Weathered coal humic acid water-holding agent not only safety, the health that the method is obtained, can degrade voluntarily, soil also not easily hardens, and improves Soil structure, makes crop water and fertilizer utilization improve more than 85%.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) dried weathered coal is put into micronizer mill to pulverize, cross 80 ~ 90 order steel sieves, obtain weathered coal particle, take 20 ~ 30g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 200 ~ 300mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 100 ~ 110 DEG C and boil 20 ~ 30min and obtain mixed solution;
(2) filter after the above-mentioned mixed solution boiled being cooled to 50 ~ 55 DEG C, filter residue deionized water rinsing carries out desalting treatment 3 ~ 5 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 100 ~ 300mL mass concentration is 30%, move into water-bath be warming up to 90 ~ 110 DEG C boil after, at room temperature leave standstill 30 ~ 50min, with horizontal high-speed centrifuge process 10 ~ 20min, centrifugal rotational speed is 4000 ~ 5000r/min, be separated and remove throw out, obtaining supernatant liquor is sodium humate solution;
(3) sodium humate solution pH to 2 ~ 3 are regulated with the sulfuric acid that mass concentration is 15%, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 6 ~ 7, filter residue is moved into baking oven, after drying at 105 ~ 110 DEG C, namely obtains humic acids;
(4) in the there-necked flask that agitator, reflux exchanger are housed, add 200 ~ 300mg sodium lauryl sulphate make dispersion agent and oil phase made by 100 ~ 200mL normal hexane, heating in water bath to 50 ~ 60 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 10 ~ 20g again, stir and obtain mixing solutions;
(5) in above-mentioned mixed solution, the acrylic acid solution that 20 ~ 50mL mass concentration is 70% is added, pH to 7 ~ 8 are regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 10 ~ 20mL mass concentration is 1% again, warming-in-water to 40 ~ 60 DEG C make it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 50 ~ 80 DEG C and continue reaction 30 ~ 60min, obtained transparence polymer gel water-holding agent first product;
(6) above-mentioned first product is put into concentration tank, 1000 ~ 1200Pa is decompressed in tank, concentrate under normal temperature and obtain pureed enriched material, again enriched material is put into baking oven to be dried with the temperature of 80 ~ 90 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 50 ~ 60 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
Application method of the present invention is: a kind of weathered coal humic acid water-holding agent obtained by the present invention is evenly sprinkling upon the surface, soil that arid treats water conservation, wherein sow 20 ~ 30g for every square metre, and stir evenly leveling by iron teeth rake comb reason, then every square metre of diversion 70 ~ 90L, can carry out sowing and applying fertilizer after irrigating for 5 ~ 10 days.Not only safety, health, can degrade voluntarily, soil also not easily hardens, and improves Soil structure, makes crop water and fertilizer utilization improve more than 85%.
The invention has the beneficial effects as follows:
(1) take weathered coal as starting material, extract Sodium salts humic acids and prepare water-loss reducer of soil, reduce production cost, indirectly improve agriculture yield;
(2) water-loss reducer of soil made, safety, health, can degrade voluntarily, and soil is not easily hardened, and be safe from harm for environment, human body;
(3) Be very effective, improves Soil structure, makes crop water and fertilizer utilization improve more than 85%.
Embodiment
First dried weathered coal is put into micronizer mill to pulverize, cross 80 ~ 90 order steel sieves, obtain weathered coal particle, take 20 ~ 30g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 200 ~ 300mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 100 ~ 110 DEG C and boil 20 ~ 30min and obtain mixed solution; Then filter after the above-mentioned mixed solution boiled being cooled to 50 ~ 55 DEG C, filter residue deionized water rinsing carries out desalting treatment 3 ~ 5 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 100 ~ 300mL mass concentration is 30%, move into water-bath be warming up to 90 ~ 110 DEG C boil after, at room temperature leave standstill 30 ~ 50min, with horizontal high-speed centrifuge process 10 ~ 20min, centrifugal rotational speed is 4000 ~ 5000r/min, be separated and remove throw out, obtaining supernatant liquor is sodium humate solution; Sodium humate solution pH to 2 ~ 3 are regulated subsequently with the sulfuric acid that mass concentration is 15%, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 6 ~ 7, filter residue is moved into baking oven, after drying at 105 ~ 110 DEG C, namely obtains humic acids; Next in the there-necked flask that agitator, reflux exchanger are housed, add 200 ~ 300mg sodium lauryl sulphate make dispersion agent and oil phase made by 100 ~ 200mL normal hexane, heating in water bath to 50 ~ 60 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 10 ~ 20g again, stir and obtain mixing solutions; The acrylic acid solution that 20 ~ 50mL mass concentration is 70% is added afterwards in above-mentioned mixed solution, pH to 7 ~ 8 are regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 10 ~ 20mL mass concentration is 1% again, warming-in-water to 40 ~ 60 DEG C make it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 50 ~ 80 DEG C and continue reaction 30 ~ 60min, obtained transparence polymer gel water-holding agent first product; Finally above-mentioned first product is put into concentration tank, 1000 ~ 1200Pa is decompressed in tank, concentrate under normal temperature and obtain pureed enriched material, again enriched material is put into baking oven to be dried with the temperature of 80 ~ 90 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 50 ~ 60 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
Example 1
First dried weathered coal is put into micronizer mill to pulverize, cross 80 order steel sieves, obtain weathered coal particle, take 20g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 200mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 100 DEG C and boil 20min and obtain mixed solution; Then filter after the above-mentioned mixed solution boiled being cooled to 50 DEG C, filter residue deionized water rinsing carries out desalting treatment 3 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 100mL mass concentration is 30%, move into water-bath be warming up to 90 DEG C boil after, at room temperature leave standstill 30min, with horizontal high-speed centrifuge process 10min, centrifugal rotational speed is 4000r/min, and be separated and remove throw out, obtaining supernatant liquor is sodium humate solution; Regulate sodium humate solution pH to 2 with the sulfuric acid that mass concentration is 15% subsequently, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 6, filter residue is moved into baking oven, after drying at 105 DEG C, namely obtain humic acids; Next in the there-necked flask that agitator, reflux exchanger are housed, add 200mg sodium lauryl sulphate make dispersion agent and oil phase made by 100mL normal hexane, heating in water bath to 50 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 10g again, stir and obtain mixing solutions; The acrylic acid solution that 20mL mass concentration is 70% is added afterwards in above-mentioned mixed solution, pH to 7 is regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 10mL mass concentration is 1% again, warming-in-water to 40 DEG C makes it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 50 DEG C and continue reaction 30min, obtained transparence polymer gel water-holding agent first product; Finally above-mentioned first product is put into concentration tank, be decompressed to 1000Pa in tank, concentratedly under normal temperature obtain pureed enriched material, then enriched material is put into baking oven and dried with the temperature of 80 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 50 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
This example operation process is simple, during operation, a kind of weathered coal humic acid water-holding agent obtained by the present invention is evenly sprinkling upon the surface, soil that arid treats water conservation, wherein sow 40g for every square metre, and stir evenly leveling by iron teeth rake comb reason, then every square metre of diversion 70L, irrigates and within latter 5 days, can carry out sowing and applying fertilizer.Not only safety, health, can degrade voluntarily, soil also not easily hardens, and improves Soil structure, makes crop water and fertilizer utilization improve 85%.
Example 2
First dried weathered coal is put into micronizer mill to pulverize, cross 85 order steel sieves, obtain weathered coal particle, take 25g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 250mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 105 DEG C and boil 25min and obtain mixed solution; Then filter after the above-mentioned mixed solution boiled being cooled to 53 DEG C, filter residue deionized water rinsing carries out desalting treatment 4 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 200mL mass concentration is 30%, move into water-bath be warming up to 105 DEG C boil after, at room temperature leave standstill 40min, with horizontal high-speed centrifuge process 15min, centrifugal rotational speed is 4500r/min, and be separated and remove throw out, obtaining supernatant liquor is sodium humate solution; Regulate sodium humate solution pH to 2.5 with the sulfuric acid that mass concentration is 15% subsequently, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 6.5, filter residue is moved into baking oven, after drying at 108 DEG C, namely obtain humic acids; Next in the there-necked flask that agitator, reflux exchanger are housed, add 250mg sodium lauryl sulphate make dispersion agent and oil phase made by 150mL normal hexane, heating in water bath to 55 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 15g again, stir and obtain mixing solutions; The acrylic acid solution that 40mL mass concentration is 70% is added afterwards in above-mentioned mixed solution, pH to 7.5 is regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 15mL mass concentration is 1% again, warming-in-water to 50 DEG C makes it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 65 DEG C and continue reaction 45min, obtained transparence polymer gel water-holding agent first product; Finally above-mentioned first product is put into concentration tank, be decompressed to 1100Pa in tank, concentratedly under normal temperature obtain pureed enriched material, then enriched material is put into baking oven and dried with the temperature of 85 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 55 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
This example operation process is simple, during operation, a kind of weathered coal humic acid water-holding agent obtained by the present invention is evenly sprinkling upon the surface, soil that arid treats water conservation, wherein sow 50g for every square metre, and stir evenly leveling by iron teeth rake comb reason, then every square metre of diversion 80L, irrigates and within latter 8 days, can carry out sowing and applying fertilizer.Not only safety, health, can degrade voluntarily, soil also not easily hardens, and improves Soil structure, makes crop water and fertilizer utilization improve 88%.
Example 3
First dried weathered coal is put into micronizer mill to pulverize, cross 90 order steel sieves, obtain weathered coal particle, take 30g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 300mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 110 DEG C and boil 30min and obtain mixed solution; Then filter after the above-mentioned mixed solution boiled being cooled to 55 DEG C, filter residue deionized water rinsing carries out desalting treatment 5 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 300mL mass concentration is 30%, move into water-bath be warming up to 110 DEG C boil after, at room temperature leave standstill 50min, with horizontal high-speed centrifuge process 20min, centrifugal rotational speed is 5000r/min, and be separated and remove throw out, obtaining supernatant liquor is sodium humate solution; Regulate sodium humate solution pH to 3 with the sulfuric acid that mass concentration is 15% subsequently, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 7, filter residue is moved into baking oven, after drying at 110 DEG C, namely obtain humic acids; Next in the there-necked flask that agitator, reflux exchanger are housed, add 300mg sodium lauryl sulphate make dispersion agent and oil phase made by 200mL normal hexane, heating in water bath to 60 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 20g again, stir and obtain mixing solutions; The acrylic acid solution that 50mL mass concentration is 70% is added afterwards in above-mentioned mixed solution, pH to 8 is regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 20mL mass concentration is 1% again, warming-in-water to 60 DEG C makes it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 80 DEG C and continue reaction 60min, obtained transparence polymer gel water-holding agent first product; Finally above-mentioned first product is put into concentration tank, be decompressed to 1200Pa in tank, concentratedly under normal temperature obtain pureed enriched material, then enriched material is put into baking oven and dried with the temperature of 90 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 60 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
This example operation process is simple, during operation, a kind of weathered coal humic acid water-holding agent obtained by the present invention is evenly sprinkling upon the surface, soil that arid treats water conservation, wherein sow 60g for every square metre, and stir evenly leveling by iron teeth rake comb reason, then every square metre of diversion 90L, irrigates and within latter 10 days, can carry out sowing and applying fertilizer.Not only safety, health, can degrade voluntarily, soil also not easily hardens, and improves Soil structure, makes crop water and fertilizer utilization improve 90%.
Claims (1)
1. a preparation method for weathered coal humic acid water-holding agent, is characterized in that concrete preparation process is:
(1) dried weathered coal is put into micronizer mill to pulverize, cross 80 ~ 90 order steel sieves, obtain weathered coal particle, take 20 ~ 30g weathered coal particle and put into 500mL beaker, add the dilute hydrochloric acid solution that 200 ~ 300mL mass concentration is 2% again, move into oil bath pan after stirring with glass stick, be warming up to 100 ~ 110 DEG C and boil 20 ~ 30min and obtain mixed solution;
(2) filter after the above-mentioned mixed solution boiled being cooled to 50 ~ 55 DEG C, filter residue deionized water rinsing carries out desalting treatment 3 ~ 5 times, afterwards filter residue is poured in 500mL beaker, add the sodium hydroxide solution that 100 ~ 300mL mass concentration is 30%, move into water-bath be warming up to 90 ~ 110 DEG C boil after, at room temperature leave standstill 30 ~ 50min, with horizontal high-speed centrifuge process 10 ~ 20min, centrifugal rotational speed is 4000 ~ 5000r/min, be separated and remove throw out, obtaining supernatant liquor is sodium humate solution;
(3) sodium humate solution pH to 2 ~ 3 are regulated with the sulfuric acid that mass concentration is 15%, produce throw out, filter afterwards and obtain filter residue, then with deionized water rinsing filter residue until its pH is 6 ~ 7, filter residue is moved into baking oven, after drying at 105 ~ 110 DEG C, namely obtains humic acids;
(4) in the there-necked flask that agitator, reflux exchanger are housed, add 200 ~ 300mg sodium lauryl sulphate make dispersion agent and oil phase made by 100 ~ 200mL normal hexane, heating in water bath to 50 ~ 60 DEG C, stirring with glass stick makes dispersion agent fully dissolve, add the above-mentioned obtained humic acids of 10 ~ 20g again, stir and obtain mixing solutions;
(5) in above-mentioned mixed solution, the acrylic acid solution that 20 ~ 50mL mass concentration is 70% is added, pH to 7 ~ 8 are regulated with the potassium hydroxide solution that mass concentration is 40% under whipped state, be cooled to room temperature and add the potassium persulfate solution that 10 ~ 20mL mass concentration is 1% again, warming-in-water to 40 ~ 60 DEG C make it that graft polymerization reaction occur, stop when mixture becomes translucent stirring, continue to be warming up to 50 ~ 80 DEG C and continue reaction 30 ~ 60min, obtained transparence polymer gel water-holding agent first product;
(6) above-mentioned first product is put into concentration tank, 1000 ~ 1200Pa is decompressed in tank, concentrate under normal temperature and obtain pureed enriched material, again enriched material is put into baking oven to be dried with the temperature of 80 ~ 90 DEG C, pulverized with high speed Universalpulverizer afterwards, cross 50 ~ 60 order steel and sieve and obtain a kind of weathered coal humic acid water-holding agent.
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| CN107057712A (en) * | 2017-04-14 | 2017-08-18 | 东南大学 | Suitable for the curing agent and production and application method of highly acid Compound Heavy Metals soil |
| 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 |
| CN111019662A (en) * | 2019-12-20 | 2020-04-17 | 华南理工大学 | Soil water-retaining agent produced by using aluminum ash and preparation method thereof |
| CN112299895A (en) * | 2020-11-06 | 2021-02-02 | 五原县沃丰生物科技有限责任公司 | Humic acid nano plant nutrient and production method thereof |
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| CN112299895A (en) * | 2020-11-06 | 2021-02-02 | 五原县沃丰生物科技有限责任公司 | Humic acid nano plant nutrient and production method thereof |
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Application publication date: 20151223 |