CN117164780B - Cellulose-humic acid type composite water-retaining agent and preparation method thereof - Google Patents
Cellulose-humic acid type composite water-retaining agent and preparation method thereof Download PDFInfo
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- CN117164780B CN117164780B CN202311157231.9A CN202311157231A CN117164780B CN 117164780 B CN117164780 B CN 117164780B CN 202311157231 A CN202311157231 A CN 202311157231A CN 117164780 B CN117164780 B CN 117164780B
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 81
- 239000004021 humic acid Substances 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000010902 straw Substances 0.000 claims abstract description 123
- 239000002361 compost Substances 0.000 claims abstract description 108
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 47
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 47
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000003999 initiator Substances 0.000 claims abstract description 31
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 65
- 238000000855 fermentation Methods 0.000 claims description 42
- 230000004151 fermentation Effects 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 38
- 239000007864 aqueous solution Substances 0.000 claims description 35
- 239000000084 colloidal system Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- 240000008042 Zea mays Species 0.000 claims description 20
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 20
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 20
- 235000005822 corn Nutrition 0.000 claims description 20
- 239000002054 inoculum Substances 0.000 claims description 19
- 230000004913 activation Effects 0.000 claims description 16
- 238000006116 polymerization reaction Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- 238000007334 copolymerization reaction Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 230000010355 oscillation Effects 0.000 claims description 13
- 230000003213 activating effect Effects 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims description 10
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 235000013312 flour Nutrition 0.000 claims description 10
- 235000019691 monocalcium phosphate Nutrition 0.000 claims description 10
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 10
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 239000005457 ice water Substances 0.000 claims description 7
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 description 25
- 239000000499 gel Substances 0.000 description 9
- 238000006386 neutralization reaction Methods 0.000 description 9
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 238000004132 cross linking Methods 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 5
- 229910052793 cadmium Inorganic materials 0.000 description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 5
- 229910052753 mercury Inorganic materials 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000010633 broth Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical group [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
Landscapes
- Fertilizers (AREA)
Abstract
The invention relates to the technical field of water-retaining agents, in particular to a cellulose-humic acid type composite water-retaining agent and a preparation method thereof. The invention provides a cellulose-humic acid type composite water-retaining agent, which comprises the following components: straw compost, dimethyl sulfoxide, a catalyst, an alkali solution, neutralizing acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide. The water-retaining agent is environment-friendly and soil-friendly, and has low cost, simple and convenient method and easy operation.
Description
Technical Field
The invention relates to the technical field of water-retaining agents, in particular to a cellulose-humic acid type composite water-retaining agent and a preparation method thereof.
Background
The water-retaining agent is also called as super absorbent resin (SAP), is a high molecular polymer with a network structure, and the high molecular water-absorbing material contains a large number of strong hydrophilic groups and is in a molecular cross-linking structure, can generally absorb water with the weight of tens to thousands times of the self weight and form hydrogel, and is widely applied to the aspects of ecological restoration, agricultural production, medical sanitation and the like, and particularly plays an important role in the treatment of environmental problems such as desertification, water and soil loss and the like.
At present, scientific research institutes at home and abroad develop a large number of experiments and researches aiming at the preparation of the water-retaining agent, the annual output of the water-retaining agent in China is more than 120 ten thousand tons, the water absorption multiple of the common agriculture and forestry water-retaining agent in the market is generally 200-700 times, and the common cellulose water-retaining agent, starch water-retaining agent, humic acid water-retaining agent and other compound water-retaining agents are strong in water absorption, but not easy to degrade and are used for industrial buildings; the starch water-retaining agent is environment-friendly but has higher cost, and is not suitable for agriculture and forestry operations; humic acid water-retaining agent is rich in organic matters and high in degradability, but has short service life and is difficult to put into the market.
The present invention has been made based on this.
Disclosure of Invention
The invention aims to provide a cellulose-humic acid type composite water-retaining agent and a preparation method thereof, wherein the water-retaining agent and the preparation method are environment-friendly, soil-friendly, low in cost, simple and convenient in method and easy to operate.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a cellulose-humic acid type composite water-retaining agent, which comprises the following components:
Straw compost, dimethyl sulfoxide, a catalyst, an alkali solution, neutralizing acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide;
The initiator is a mixture of potassium persulfate and sodium thiosulfate, and the mass ratio of the potassium persulfate to the sodium thiosulfate is 2-5:1-3;
the catalyst is a potassium hydroxide aqueous solution with the mass concentration of 1-3%;
the alkali solution is potassium hydroxide aqueous solution with the mass concentration of 0.5-3%;
preferably, the mass volume ratio of the straw compost to the dimethyl sulfoxide is 1-3 g: 3-7 ml;
the mass volume ratio of the straw compost to the catalyst is 1-3 g: 20-30 ml;
the mass volume ratio of the straw compost to the alkali solution is 1-3 g: 40-60 ml;
the mass volume ratio of the straw compost to the neutralization acrylic acid is 1-3 g: 2-11 ml;
the mass ratio of the straw compost to the acrylamide is 1-3: 0.5 to 5.0;
The mass ratio of the straw compost to the initiator is 1-3: 0.22 to 0.42;
the mass ratio of the straw compost to the N, N' -methylene bisacrylamide is 1-3: 0.01 to 0.09;
preferably, the preparation method of the neutralization acrylic acid comprises the following steps: mixing acrylic acid with potassium hydroxide aqueous solution in ice water bath to obtain neutralized acrylic acid;
The mass concentration of the potassium hydroxide aqueous solution is 8-12%.
The volume ratio of the acrylic acid to the potassium hydroxide aqueous solution is 1-3:3-7;
preferably, the preparation method of the straw compost comprises the following steps:
1) Mixing the straw with a fermentation inoculant, corn flour, urea and calcium superphosphate to obtain a mixed material;
2) Adjusting the water content of the mixed material to 50-70%, and stacking and fermenting for 8-12 d to obtain a fermentation product;
3) Airing the fermentation product until the water content is 10-20%, so as to obtain straw compost;
In the step 1), the length of the straw is 2-5 cm; the fermentation inoculant is BFA fermentation inoculant; the mass ratio of the mixture of the straw and the fermentation inoculant is 250-1000:1; the mass ratio of the mixture of the straw and the urea is 60-200:1; the mass ratio of the mixture of the straw and the calcium superphosphate is 6-20:1; the mass ratio of the fermentation inoculant to the corn flour is 1:8-12; the temperature of the stacking fermentation is 60-65 ℃;
preferably, the straw in step 1) is corn straw.
The invention also provides a preparation method of the cellulose-humic acid type composite water-retaining agent, wherein the preparation method is an aqueous solution copolymerization method or a microwave polymerization method;
Preferably, the aqueous solution copolymerization method comprises the steps of:
(1) Mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
(2) Mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
(3) Activating the reinforced straw compost in a water bath to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 25-35 min to obtain black colloid;
(5) Ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
The water bath activation temperature is 65-85 ℃, and the water bath activation time is 30-60 min;
The heating is water bath heating; the heating temperature is 70-90 ℃;
The temperature of the drying is 40-60 ℃;
preferably, the microwave polymerization method comprises the steps of:
Step 1: mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
step 2: mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
step 3: activating the reinforced straw compost by microwaves to obtain activated reinforced straw compost;
Step 4: mixing the activated reinforced straw compost with the neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 5-15 min to obtain black colloid;
step 5: ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
the power of the microwave activation is 210-450W, the time of the microwave activation is 5-20 min,
The heating is microwave heating; the heating power is 400-450W;
the temperature of the drying is 40-60 ℃.
The invention has the beneficial effects that:
The invention provides a cellulose-humic acid type composite water-retaining agent, which takes straw compost as raw materials of humic acid and cellulose, optimizes the process of the cellulose-humic acid type composite water-retaining agent, and ensures that indexes such as water absorption multiple, brine absorption multiple, moisture, cadmium (calculated by elements), chromium (calculated by elements), mercury (calculated by elements), lead (calculated by elements), arsenic (calculated by elements) and the like all meet the standards of NY/T886-2022, has high content of potassium elements and is environment-friendly. The cellulose-humic acid type composite water-retaining agent has rich compost humic acid in raw materials, and the humic acid is also a main component of soil organic substances, so that the water-retaining agent has higher soil friendliness. The corn straw compost is used as a raw material for preparing the cellulose-humic acid type composite water-retaining agent, so that a reference can be provided for straw recycling in China, and a theoretical basis is provided for preparing the cellulose-humic acid type composite water-retaining agent.
The invention also provides a preparation method of the cellulose-humic acid type composite water-retaining agent, which utilizes the hydroxyl in the polarization compost of dimethyl sulfoxide polar solution and KOH solution (serving as an alkaline catalyst) to greatly increase the subsequent graft copolymerization capability of cellulose humic acid, and then the cellulose-humic acid type composite water-retaining agent is polymerized with acrylic acid and acrylamide type monomers under the action of a cross-linking agent to form a three-dimensional network water-retaining structure to obtain the water-retaining agent; adding potassium hydroxide solution with a certain concentration for oscillation, so that humic acid in the compost is dissolved in alkali liquor to be in a free state and then participates in copolymerization reaction; the acrylic acid and the acrylamide have strong hydrophilicity and grafting activity, and a proper amount of the acrylic acid and the acrylamide can increase the grafting rate and the length of branched chains, accelerate the polymerization reaction rate, contribute to the formation of a cross-linked grid structure, improve the gel strength and macroscopically reflect the increase of the water absorption multiple; the excessive grafting chain is too compact, the gap of the crosslinked network structure is small, and meanwhile, the monomer which does not participate in polymerization can be wrapped by the tightly-formed network structure and is difficult to participate in subsequent reaction, so that the monomer is blocked in the space structure, and the water absorption multiple of the product is reduced; the cross-linking agent is N, N' -methylene bisacrylamide, the cross-linking degree of the copolymer is low when the consumption is low, a stable network cross-linking structure is difficult to form, and the water absorption capacity is weak; and when the dosage is too high, the crosslinking degree is high, the network structure is compact, and the water absorption expansion of the product is not facilitated; under the proper water bath temperature, the reaction activity is strong, the monomers of the grafting monomer, the cross-linking agent and the initiator are fully contacted to form more cross-linking points, the cross-linking structure is perfect, the polymerization speed is accelerated, and the water absorption multiple of the product can be effectively improved. When the temperature is less than 60 ℃, the reaction does not occur, a water-retaining agent cannot be generated, and when the temperature exceeds 90 ℃, the graft chain of the graft copolymer is shortened due to the fact that the graft chain is easily subjected to polymerization, the polymerization reaction is uneven, and the water absorption multiple of the product is reduced.
Detailed Description
The invention provides a cellulose-humic acid type composite water-retaining agent, which comprises the following components:
Straw compost, dimethyl sulfoxide, a catalyst, an alkali solution, neutralizing acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide;
the initiator is a mixture of potassium persulfate and sodium thiosulfate, and the mass ratio of the potassium persulfate to the sodium thiosulfate is 2-5:1-3, preferably 3.5:2;
the catalyst is a potassium hydroxide aqueous solution with the mass concentration of 1-3%, preferably 2%;
The alkali solution is potassium hydroxide aqueous solution with the mass concentration of 0.5-3%, preferably 1.5-2%, and more preferably 1.75%;
In the invention, the mass volume ratio of the straw compost to the dimethyl sulfoxide is 1-3 g:3 to 7ml, preferably 2g:5ml;
the mass volume ratio of the straw compost to the catalyst is 1-3 g: 20-30 ml, preferably 2g:25ml;
The mass volume ratio of the straw compost to the alkali solution is 1-3 g: 40-60 ml, preferably 2g:50ml;
The mass volume ratio of the straw compost to the neutralization acrylic acid is 1-3 g: 2-11 ml, preferably 2g:6.5ml;
The mass ratio of the straw compost to the acrylamide is 1-3: 0.5 to 5.0, preferably 2:2.75;
The mass ratio of the straw compost to the initiator is 1-3: 0.22 to 0.42, preferably 2:0.32;
the mass ratio of the straw compost to the N, N' -methylene bisacrylamide is 1-3: 0.01 to 0.09, preferably 2:0.05;
in the invention, the preparation method of the neutralization acrylic acid comprises the following steps: mixing acrylic acid with potassium hydroxide aqueous solution in ice water bath to obtain neutralized acrylic acid;
the mass concentration of the potassium hydroxide aqueous solution is 8-12%, preferably 10%;
The volume ratio of the acrylic acid to the potassium hydroxide aqueous solution is 1-3:3-7, preferably 2:5;
in the invention, the preparation method of the straw compost comprises the following steps:
1) Mixing the straw with a fermentation inoculant, corn flour, urea and calcium superphosphate to obtain a mixed material;
2) Adjusting the water content of the mixed material to 50-70%, and stacking and fermenting for 8-12 d to obtain a fermentation product;
3) Airing the fermentation product until the water content is 10-20%, so as to obtain straw compost;
In the step 1), the length of the straw is 2-5 cm, preferably 3cm; the fermentation inoculant is BFA fermentation inoculant; the mass ratio of the mixture of the straw and the fermentation inoculant is 250-1000:1; preferably 500 to 750:1, more preferably 625:1; the mass ratio of the straw to the urea is 60-200:1, preferably 100-160:1, and more preferably 130:1; the mass ratio of the straw to the calcium superphosphate is 6-20:1, preferably 10-16:1, and further preferably 13:1; the mass ratio of the fermentation inoculant to the corn flour is 1:8-12, preferably 1:10; the temperature of the stacking fermentation is 60-65 ℃, preferably 62.5; the water content is preferably 60%; the fermentation time is preferably 10d;
the water content in step 3) is preferably 15%;
In the invention, the straw in the step 1) is corn straw;
The invention also provides a preparation method of the cellulose-humic acid type composite water-retaining agent, which is an aqueous solution copolymerization method or a microwave polymerization method.
In the present invention, the aqueous solution copolymerization method comprises the steps of:
(1) Mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
(2) Mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
(3) Activating the reinforced straw compost in a water bath to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 25-35 min to obtain black colloid;
(5) Ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
In the present invention, the time of the standing in the step (1) is preferably 9 to 11 minutes, more preferably 10 minutes;
The temperature of the oscillation is 25-35 ℃, preferably 29-31 ℃, and more preferably 30 ℃; the time of the oscillation is 15 to 25min, preferably 19 to 21min, and more preferably 20min;
The water bath activation temperature is 65-85 ℃, preferably 70-80 ℃, more preferably 75 ℃, and the water bath activation time is 30-60 min, preferably 40-50 min, more preferably 45min;
the heating is water bath heating; the heating temperature is 70-90 ℃, preferably 78-82 ℃, and more preferably 80 ℃; the heating time is preferably 30 minutes.
The temperature of the drying is 40 to 60 ℃, preferably 45 to 55 ℃, and more preferably 50 ℃.
In the present invention, the microwave polymerization method comprises the steps of:
step 1: mixing straw compost, dimethyl sulfoxide and an alkaline catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
step 2: mixing the filter residue with potassium hydroxide aqueous solution, and oscillating to obtain reinforced straw compost;
step 3: activating the reinforced straw compost by microwaves to obtain activated reinforced straw compost;
Step 4: mixing the activated reinforced straw compost with the neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 5-15 min to obtain black colloid;
step 5: ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
in the present invention, the time of the standing in the step 1 is preferably 9 to 11 minutes, more preferably 10 minutes;
The temperature of the oscillation is 25-35 ℃, preferably 29-31 ℃, and more preferably 30 ℃; the time of the oscillation is 15 to 25min, preferably 19 to 21min, and more preferably 20min;
The microwave activation power is 210-450W, preferably 310-350W, and more preferably 330W; the microwave activation time is 5-20 min, preferably 10-15 min, and more preferably 12.5min;
The heating is microwave heating; the heating power is 400-450W, preferably 420-430W, more preferably 425W; the heating time is preferably 10 minutes.
The temperature of the drying is 40 to 60 ℃, preferably 45 to 55 ℃, and more preferably 50 ℃.
In the present invention, BFA fermentation broths are purchased from Fujian oasis Biochemical Co.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the straw compost comprises the following steps:
1) Drying 1000Kg of corn stalks, crushing the corn stalks into sections with the length of 2cm, adding 2Kg of BFA fermentation inoculant, 20Kg of corn flour, 10Kg of urea and 100Kg of calcium superphosphate, and mixing to obtain a mixed material;
2) Regulating the water content of the mixed material to 60%, piling, covering the surface with a nano bio-compost film, and carrying out mixed fermentation at 63 ℃ for 10d to obtain a fermentation product;
3) And airing the fermentation product until the water content is 15%, and obtaining the straw compost.
The preparation method of the neutralization acrylic acid comprises the following steps:
4ml of acrylic acid and 14ml of 10% aqueous potassium hydroxide solution were mixed and allowed to stand in an ice water bath for 20 minutes to obtain neutralized acrylic acid.
The preparation method of the initiator comprises the following steps:
The potassium persulfate and the sodium thiosulfate are mixed according to the mass ratio of 3:1 to prepare the initiator.
The preparation of the cellulose-humic acid type composite water-retaining agent by an aqueous solution copolymerization method comprises the following steps:
(1) Mixing 2g of straw compost, 5ml of dimethyl sulfoxide and 25ml of 2% potassium hydroxide aqueous solution, standing for 10min, and carrying out suction filtration to obtain filter residues;
(2) 100ml of 1.5% potassium hydroxide aqueous solution is added into the filter residue, and the mixture is oscillated for 20min at 30 ℃ to obtain the reinforced straw compost.
(3) Activating the reinforced straw compost in a water bath at 80 ℃ for 30min to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with 18ml of neutralizing acrylic acid, 1g of acrylamide, 0.68g of initiator and 0.04g of N, N' -methylene bisacrylamide, and heating in a water bath at 80 ℃ for 30min to obtain black colloid;
(5) And (3) ultrasonically cleaning the black colloid for 5 minutes at 30 ℃, and drying the black colloid at 50 ℃ to obtain the cellulose-humic acid type composite water-retaining agent.
Example 2
A preparation method of reinforced straw compost comprises the following steps:
1) Drying and crushing 300Kg corn stalks into sections with the length of 2cm, adding 1.2Kg BFA fermentation inoculant, 14.4Kg corn flour, 5Kg urea and 30Kg calcium superphosphate, and mixing to obtain a mixed material;
2) Regulating the water content of the mixed material to 55%, piling, covering the surface with a nano bio-compost film, and carrying out mixed fermentation at 60 ℃ for 12d to obtain a fermentation product;
3) And airing the fermentation product until the water content is 17%, and obtaining the straw compost.
The preparation method of the neutralization acrylic acid comprises the following steps:
4ml of acrylic acid and 13.6ml of a 12% aqueous potassium hydroxide solution were mixed, and the mixture was allowed to stand in an ice water bath for 20 minutes to obtain a neutralized acrylic acid.
The preparation method of the initiator comprises the following steps:
The potassium persulfate and the sodium thiosulfate are mixed according to the mass ratio of 3:1 to prepare the initiator.
The preparation of the cellulose-humic acid type composite water-retaining agent by an aqueous solution copolymerization method comprises the following steps:
(1) Mixing 3g of straw compost, 6ml of dimethyl sulfoxide and 30ml of 2% potassium hydroxide aqueous solution, standing for 12min, and suction filtering to obtain filter residues;
(2) Adding 165ml of 2.46% potassium hydroxide aqueous solution into the filter residue, and oscillating at 25 ℃ for 25min to obtain reinforced straw compost;
(3) Activating the reinforced straw compost in water bath at 85 ℃ for 48.8min to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with 26.4ml of neutralizing acrylic acid, 4.47g of acrylamide, 0.78g of initiator and 0.06g of N, N' -methylene bisacrylamide, and heating in a water bath at 90 ℃ for 25min to obtain black colloid;
(5) And (3) ultrasonically cleaning the black colloid for 5 minutes at 30 ℃, and drying at 60 ℃ to obtain the cellulose-humic acid type composite water-retaining agent.
Example 3
The preparation method of the reinforced straw compost comprises the following steps:
1) Drying 1000Kg of corn stalks, crushing the corn stalks into sections with the length of 2cm, adding 2Kg of BFA fermentation inoculant, 20Kg of corn flour, 10Kg of urea and 100Kg of calcium superphosphate, and mixing to obtain a mixed material;
2) Regulating the water content of the mixed material to 60%, piling, covering the surface with a nano bio-compost film, and carrying out mixed fermentation at 63 ℃ for 10d to obtain a fermentation product;
3) And airing the fermentation product until the water content is 15%, and obtaining the straw compost.
The preparation method of the neutralization acrylic acid comprises the following steps:
4ml of acrylic acid and 12ml of 11% aqueous potassium hydroxide solution were mixed and allowed to stand in an ice water bath for 20 minutes to obtain neutralized acrylic acid.
The preparation method of the initiator comprises the following steps:
The potassium persulfate and the sodium thiosulfate are mixed according to the mass ratio of 3:1 to prepare the initiator.
The preparation of the cellulose-humic acid type composite water-retaining agent by a microwave polymerization method comprises the following steps:
(1) Mixing 2g of straw compost, 5ml of dimethyl sulfoxide and 25ml of 2% potassium hydroxide aqueous solution, standing for 10min, and carrying out suction filtration to obtain filter residues;
(2) Adding 100ml of 1.5% potassium hydroxide aqueous solution into the filter residue, and oscillating for 20min at 30 ℃ to obtain reinforced straw compost;
(3) Microwave activating the reinforced straw compost for 5min at 350W to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with 16ml of neutralizing acrylic acid, 8g of acrylamide, 0.6g of initiator and 0.04g of N, N' -methylene bisacrylamide, and heating by 420W microwaves for 10min to obtain black colloid;
(5) And ultrasonically cleaning the black colloid for 5 minutes at 30 ℃ and drying the black colloid at 50 ℃ to obtain the cellulose-humic acid type composite water-retaining agent.
Example 4
A preparation method of reinforced straw compost comprises the following steps:
1) Drying and crushing 300Kg corn stalks into sections with the length of 2cm, adding 1.2Kg BFA fermentation inoculant, 14.4Kg corn flour, 5Kg urea and 30Kg calcium superphosphate, and mixing to obtain a mixed material;
2) Regulating the water content of the mixed material to 55%, piling, covering the surface with a nano bio-compost film, and carrying out mixed fermentation at 60 ℃ for 12d to obtain a fermentation product;
3) Airing the fermentation product until the water content is 17%, and obtaining straw compost;
the preparation method of the neutralization acrylic acid comprises the following steps:
4ml of acrylic acid and 11.6ml of a 10% aqueous potassium hydroxide solution were mixed, and the mixture was allowed to stand in an ice water bath for 20 minutes to obtain a neutralized acrylic acid.
The preparation method of the initiator comprises the following steps:
The potassium persulfate and the sodium thiosulfate are mixed according to the mass ratio of 3:1 to prepare the initiator.
The preparation of the cellulose-humic acid type composite water-retaining agent by a microwave polymerization method comprises the following steps:
(1) Mixing 3g of straw compost, 6ml of dimethyl sulfoxide and 30ml of 2% potassium hydroxide aqueous solution, standing for 12min, and suction filtering to obtain filter residues;
(2) Adding 165ml of 2.46% potassium hydroxide aqueous solution into the filter residue, and oscillating at 25 ℃ for 25min to obtain reinforced straw compost;
(3) Activating the reinforced straw compost at 210W for 14.4min to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with 23.4ml of neutralizing acrylic acid, 12.0g of acrylamide, 0.66g of initiator and 0.06g of N, N' -methylene bisacrylamide, and heating by 400W microwaves for 12min to obtain black colloid;
(5) And (3) ultrasonically cleaning the black colloid for 5 minutes at 30 ℃, and drying at 60 ℃ to obtain the cellulose-humic acid type composite water-retaining agent.
Experimental example 1
The cellulose-humic acid type composite water-retaining agent prepared in examples 1 to 4 was subjected to performance test. The test index comprises water absorption times, brine absorption times, mercury, arsenic, cadmium, lead, chromium, potassium, organic matter content and pH. The specific test method is as follows:
The measuring method comprises the following steps:
Determination of the water absorption capacity: 1g of the cellulose-humic acid type composite water-retaining agent of examples 1-4 is respectively weighed, mixed and stirred with water for 5min, kept stand at room temperature for 24h to obtain gel, the gel is poured into a 80-mesh sieve, the sieve is horizontally placed for 10min, and the cellulose-humic acid type composite water-retaining agent is obliquely placed for 10min and weighed, so that the water absorption multiple of the cellulose-humic acid type composite water-retaining agent is calculated.
The water absorption multiple is calculated according to the following formula:
Wherein Q: water absorption multiple (g/g) of the water-retaining agent; m 1: gel mass after water absorption (g); m 2 mass (g) of water-retaining agent.
Determination of the salt absorption fold: 1g of the cellulose-humic acid type composite water-retaining agent of examples 1-4 and 0.9% NaCl solution are respectively weighed, mixed and stirred for 5min, and kept stand for 24h at room temperature to obtain gel, the gel is poured into a 80-mesh sieve, the sieve is placed horizontally for 10min, then the gel is placed obliquely for 10min, the gel weight is weighed, and the salt absorption multiple of the water-retaining agent is calculated.
The water-retaining agent salt water absorption multiple is calculated according to the following formula:
Wherein: v: the water-retaining agent absorbs saline multiple (g/g); m 1: gel mass (g) after saline absorption; m 2 mass (g) of water-retaining agent.
The water absorption multiple, the salt water absorption multiple and the pH of the water-retaining agent are measured according to NY/T886-2022 standard; determining the content of organic matters, referring to the NY/T525-2021 standard of the organic fertilizer, oxidizing the water-retaining agent by potassium dichromate, and titrating by using ferrous ammonium sulfate; the determination of the mercury, arsenic, cadmium, lead and chromium of the water-retaining agent refers to the determination standard of the mercury, arsenic, cadmium, lead and chromium of the NY/T1978-2022 fertilizer, and the total potassium content of the water-retaining agent refers to the determination standard of the potassium content of the NY/T2540-2014 fertilizer. The test results are shown in Table 1.
TABLE 1 cellulose-humic acid type composite Water retaining agent related Properties
The cellulose-humic acid type composite water-retaining agent obtained by the aqueous solution copolymerization method and the microwave polymerization method meets the NY/T886-2022 standard in terms of indexes such as water absorption multiple, salt absorption multiple, moisture, cadmium (calculated by elements), chromium (calculated by elements), mercury (calculated by elements), lead (calculated by elements), arsenic (calculated by elements) and the like, has weak acidity of pH 5.5 and organic matters of 46.1-46.4 percent. In the process of preparing the water-retaining agent by the method, KOH is adopted for pretreatment, strengthening grafting functional groups and acrylic acid neutralization, the potassium content of the water-retaining agent reaches 18.05% -20.00%, the water-retaining agent is a potassium salt type water-retaining agent, potassium is one of three nutritional elements required by plants, and the product can provide potassium elements for plants and enable the plants to grow.
From the above embodiments, the invention provides a cellulose-humic acid type composite water-retaining agent and a preparation method thereof, which effectively solve the problems of environmental friendliness, low cost, simple method and easy operation.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The cellulose-humic acid type composite water-retaining agent is characterized by comprising the following components:
Straw compost, dimethyl sulfoxide, a catalyst, an alkali solution, neutralizing acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide;
The initiator is a mixture of potassium persulfate and sodium thiosulfate, and the mass ratio of the potassium persulfate to the sodium thiosulfate is 2-5:1-3;
the catalyst is a potassium hydroxide aqueous solution with the mass concentration of 1-3%;
the alkali solution is potassium hydroxide aqueous solution with the mass concentration of 0.5-3%;
the mass volume ratio of the straw compost to the dimethyl sulfoxide is 1-3 g: 3-7 ml;
the mass volume ratio of the straw compost to the catalyst is 1-3 g: 20-30 ml;
the mass volume ratio of the straw compost to the alkali solution is 1-3 g: 40-60 ml;
The mass volume ratio of the straw compost to the neutralized acrylic acid is 1-3 g:2-11 ml;
the mass ratio of the straw compost to the acrylamide is 1-3:0.5-5.0;
the mass ratio of the straw compost to the initiator is 1-3:0.22-0.42;
The mass ratio of the straw compost to the N, N' -methylene bisacrylamide is 1-3: 0.01 to 0.09;
The preparation method of the straw compost comprises the following steps:
1) Mixing the straw with a fermentation inoculant, corn flour, urea and calcium superphosphate to obtain a mixed material;
2) Adjusting the water content of the mixed material to 50-70%, and stacking and fermenting for 8-12 d to obtain a fermentation product;
3) Airing the fermentation product until the water content is 10-20%, so as to obtain straw compost;
In the step 1), the length of the straw is 2-5 cm; the fermentation inoculant is BFA fermentation inoculant; the mass ratio of the mixture of the straw and the fermentation inoculant is 250-1000:1; the mass ratio of the mixture of the straw and the urea is 60-200:1; the mass ratio of the mixture of the straw and the calcium superphosphate is 6-20:1; the mass ratio of the fermentation inoculant to the corn flour is 1:8-12; the temperature of the stacking fermentation is 60-65 ℃;
The preparation method of the cellulose-humic acid type composite water-retaining agent is an aqueous solution copolymerization method or a microwave polymerization method;
the aqueous solution copolymerization method comprises the following steps:
(1) Mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
(2) Mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
(3) Activating the reinforced straw compost in a water bath to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 25-35 min to obtain black colloid;
(5) Ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
the temperature of the oscillation is 25-35 ℃; the time of oscillation is 15-25 min;
The water bath activation temperature is 65-85 ℃, and the water bath activation time is 30-60 min;
The heating is water bath heating; the heating temperature is 70-90 ℃;
The temperature of the drying is 40-60 ℃;
The microwave polymerization method comprises the following steps:
Step 1: mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
step 2: mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
step 3: activating the reinforced straw compost by microwaves to obtain activated reinforced straw compost;
Step 4: mixing the activated reinforced straw compost with the neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 5-15 min to obtain black colloid;
step 5: ultrasonically cleaning the black colloid and drying to obtain a cellulose-humic acid type composite water-retaining agent;
the temperature of the oscillation is 25-35 ℃; the time of oscillation is 15-25 min;
the power of the microwave activation is 210-450W, and the time of the microwave activation is 5-20 min;
the heating is microwave heating; the heating power is 400-450W;
the temperature of the drying is 40-60 ℃.
2. The cellulose-humic acid type composite water-retaining agent according to claim 1, wherein the preparation method of the neutralized acrylic acid is as follows: mixing acrylic acid with potassium hydroxide aqueous solution in ice water bath to obtain neutralized acrylic acid;
The mass concentration of the potassium hydroxide aqueous solution is 8-12%;
The volume ratio of the acrylic acid to the potassium hydroxide aqueous solution is 1-3:3-7.
3. The cellulose-humic acid type composite water retaining agent according to claim 2 wherein the straw in step 1) is corn straw.
4. The method for preparing a cellulose-humic acid type composite water-retaining agent according to any one of claims 1 to 3, wherein the preparation method is an aqueous solution copolymerization method or a microwave polymerization method.
5. The method for preparing a cellulose-humic acid type composite water retaining agent according to claim 4 wherein the aqueous solution copolymerization method comprises the steps of:
(1) Mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
(2) Mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
(3) Activating the reinforced straw compost in a water bath to obtain activated reinforced straw compost;
(4) Mixing the activated reinforced straw compost with neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 25-35 min to obtain black colloid;
(5) And (3) ultrasonically cleaning and drying the black colloid to obtain the cellulose-humic acid type composite water-retaining agent.
6. The method for preparing a cellulose-humic acid type composite water retaining agent according to claim 5 wherein the temperature of the oscillation is 25 to 35 ℃; the time of oscillation is 15-25 min;
The water bath activation temperature is 65-85 ℃, and the water bath activation time is 30-60 min;
The heating is water bath heating; the heating temperature is 70-90 ℃;
the temperature of the drying is 40-60 ℃.
7. The method for preparing a cellulose-humic acid type composite water retaining agent according to claim 4 wherein the microwave polymerization method comprises the steps of:
Step 1: mixing straw compost, dimethyl sulfoxide and a catalyst, standing for 5-15 min, and carrying out suction filtration to obtain filter residues;
step 2: mixing the filter residue with the alkali solution, and oscillating to obtain reinforced straw compost;
step 3: activating the reinforced straw compost by microwaves to obtain activated reinforced straw compost;
Step 4: mixing the activated reinforced straw compost with the neutralized acrylic acid, acrylamide, an initiator and N, N' -methylene bisacrylamide, and heating for 5-15 min to obtain black colloid;
Step 5: and (3) ultrasonically cleaning and drying the black colloid to obtain the cellulose-humic acid type composite water-retaining agent.
8. The method for preparing a cellulose-humic acid type composite water retaining agent according to claim 7 wherein the temperature of the oscillation is 25 to 35 ℃; the time of oscillation is 15-25 min;
the power of the microwave activation is 210-450W, and the time of the microwave activation is 5-20 min;
the heating is microwave heating; the heating power is 400-450W;
the temperature of the drying is 40-60 ℃.
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