CN100554329C - The nanometer-submicron level PVA mixed polymer as fertilizer cementing coating agent preparation method - Google Patents
The nanometer-submicron level PVA mixed polymer as fertilizer cementing coating agent preparation method Download PDFInfo
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- CN100554329C CN100554329C CNB2004100913158A CN200410091315A CN100554329C CN 100554329 C CN100554329 C CN 100554329C CN B2004100913158 A CNB2004100913158 A CN B2004100913158A CN 200410091315 A CN200410091315 A CN 200410091315A CN 100554329 C CN100554329 C CN 100554329C
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Abstract
Selecting polyvinyl alcohol and polyacrylamide for use is raw material, be mixed in proportion with polyacrylamide solution after polyvinyl alcohol and the aldehyde condensation reaction, adopt microemulsified and high shear process, the PVA mixed polymers solution of preparation nano-micron, be used for the coating agent of the jointing compound and the enveloped slow release fertilizer of felted slow-release fertilizer material, inorganic slow-release fertilizer and organic-inorganic compound type slow release fertilizer all can use, and also can be used for the soil drought-relief agent of dry crop.
Description
The invention belongs to agricultural, ecotope field.
Since the nineties in 20th century, slow release fertilizer research both at home and abroad and production develop rapidly, wherein, enveloped slow release fertilizer is occupied an leading position, organic polymer material is in the great majority again in the coating agent, is characterized in an organic solvent dissolving and diluting, and production cost is higher.The developing direction of slow release fertilizer is that Envelope type combines with felted, and inorganic slow-release fertilizer combines with the organic and inorganic slow-release fertilizer.Coating cementing agent develops to fat-soluble and water-soluble direction of laying equal stress on.
The objective of the invention is to prepare and a kind ofly not only can be used as slow release fertilizer envelope agent, but also can be used as the water-soluble glued coating agent of felted slow-release fertilizer material jointing compound.
Principle of the present invention is with polyvinyl alcohol dissolving, aldehyde condensation, the polyacrylamide amine solvent, two kinds of solution is mixed in proportion, emulsification, again by high-shear (20,000 r/min), promptly become nanometer-submicron level PVA-polyacrylamide and mix polymers, be called for short nanometer-submicron level PVA mixed polymers, be used for slow release fertilizer jointing compound and coating agent.
Detailed description of the present invention:
Accompanying drawing 1 is seen in 1 technical process
2 main technique routes
2.1 the preparation of emulsifying agent
2.1.1 proportioning raw materials
| Raw material | Quality (kg) | Account for quality (%) |
| The industry water purification | 1000 | |
| Fat alcohol polyethylene ether sodium sulfate | 80～100 | 8～10 |
| Sodium dodecylbenzene sulfonate | 150～200 | 15～20 |
| Coconut acid diethanolamide | 40～50 | 4～5 |
| Castor oil polyoxyethylene ether | 40～50 | 4～5 |
| Industrial spirit (95%) | 20～30 | 2～3 |
2.1.2 operation
(1) add industrial water purification in reactor, be heated to 45 ℃～50 ℃ (being no more than 50 ℃), start agitator, slowly add fat alcohol polyethylene ether sodium sulfate, add-on is 8%～10% of a quality (down together), to dissolving fully;
(2) keep 40～50 ℃ of temperature, add Sodium dodecylbenzene sulfonate under continuously stirring, add-on is 15%～20%, to dissolving fully;
(3) add castor oil polyoxyethylene ether, add-on is 4%～5%, to dissolving fully;
(4) add coconut acid diethanolamide, add-on is 4%～5%, to dissolving fully;
(5) be cooled to below 40 ℃, add industrial spirit (95%), add-on is 2%～3%, stirs;
(6) measure the pH value, regulate pH value to 7.0～7.5, promptly become the emulsifying agent finished product with dilute sulphuric acid.
2.2 the preparation of polyvinyl formal solution
2.2.1 proportioning raw materials
| Raw material | Quality (kg) | Account for quality (%) |
| The industry water purification | 1000 | |
| Polyvinyl alcohol | 100～150 | 10～15 |
| Formaldehyde (36%～37%) | 40～60 | 4～6 |
| HCl(30％) | In right amount | |
| NaOH | In right amount | |
| Urea | 20～30 | 2～3 |
2.2.2 operation
(1) add industrial water purification in reactor, be heated to 90 ℃～95 ℃, start agitator, slowly add polyvinyl alcohol, add-on is 10%～15% of a quality (down together), maintains the temperature at more than 90 ℃, to all dissolvings;
(2) after polyvinyl alcohol all dissolves, be cooled to about 70 ℃, add rare HCl and regulate pH value to 2.0;
(3) add formaldehyde solution, add-on 4%～6%, reaction times 30～35min stops hot water circulation;
(4) add 2%～3% aqueous solution of urea, generate methylolurea, till can't smell the formaldehyde flavor with unnecessary formaldehyde;
(5) regulate pH value to 7.0～7.5 with the NaOH aqueous solution, promptly become polyvinyl formal solution.
2.3 polyacrylamide solution preparation
Add industrial water purification in reactor, be heated to 50 ℃～60 ℃ (being no more than 60 ℃), slowly add anion-polyacrylamide (molecular weight 400～6,000,000), add-on is 2%～2.5% of a quality, to dissolving fully, promptly becomes polyacrylamide solution.
2.4 the preparation of nanometer-submicron level PVA mixed polymers
(1) polyvinyl formal solution is mixed by mass ratio with polyacrylamide solution at 2: 1, start agitator, till mixing.
(2) add emulsifying agent, add-on is 5%～10% of an above-mentioned mixing solutions quality, stirs to make its complete emulsification, promptly becomes polyvinyl formal-polyacrylamide mix emulsion fluid.
(3) polyvinyl formal-polyacrylamide mix emulsion fluid is put into High shear device, 20,000 r/min speed down cuts, 5～10min, promptly become nanometer-submicron level PVA formal-polyacrylamide and mix the polymers aqueous solution (seeing accompanying drawing 2), be called for short nanometer-submicron level PVA mixed polymers.
3, High shear device
This equipment is mainly by form (seeing accompanying drawing 3) with lower member:
(1) motor: Jiangsu star-wheel high-speed electric expreess locomotive device fabrication company makes.
(2) cutter shaft and high-shear cutter: adopt the processing and manufacturing of high chrome high-nickel austenitic stainless steel material, shear knife is a spination.Cutter shaft is connected with motor output shaft by three-jaw chuck.
(3) stainless steel tank body: diameter 500mm, high 700mm.
(4) guide shell: in be lining in the effect that water conservancy diversion is played at tank body middle part, make material be turbulence state circulation high-shear, barrel diameter 200mm, high 350mm.
(5) capping: the stainless steel cover periphery reaches and is coupling to touch partly and all is stained with sealing-ring, plays airtight effect.
(6) feed inlet and outlet: opening for feed is positioned at tank body top, and discharge port is positioned at the tank body bottom.
4, the use of nanometer-submicron level PVA mixed polymers
(1) jointing compound: be used for gluing (bonding) agent of gluing (viscose glue) type slow release fertilizer, usage quantity 10～15kg/t butt fertilizer, under stirring condition, the water that adds 9 times of jointing compound quality is diluted to back use (extension rate is decided on the raw material water content) about 10 times.
(2) coating agent: be used for granular urea and composite fertilizer's coating agent, usage quantity 10～15kg/t butt fertilizer uses after the water that adding coating agent quality is 2～3 times is diluted to 3～4 times.
Advantage of the present invention:
1, nanometer-submicron level PVA mixed polymers is a full water-soluble, not with an organic solvent, has reduced production cost, and environmentally safe is one of developing direction of slow release fertilizer.
2, this mixed polymers both can be used as the coating agent of slow release fertilizer, can be used as the jointing compound of felted slow-release fertilizer material again; Both can use pure fertilizer to produce slow release fertilizer, also can be used for producing organic and inorganic compound type slow release fertilizer.
3, biological test result, the slow release fertilizer that uses this mixed polymers production is emerged to crop does not have influence, and soil microorganisms is not had any restraining effect.
4, this mixed polymers has improving effect to Soil structure, and can increase the preserving soil moisture ability.
Embodiment 1:
Production process was divided into for four steps, i.e. the preparation of the preparation of the preparation of emulsifying agent, polyvinyl formal solution, polyacrylamide solution preparation and nanometer-submicron level PVA mixed polymers.
1, the preparation of emulsifying agent
In reactor, add industrial water purification 1000kg, be heated to 45 ℃～50 ℃ (being no more than 50 ℃), start agitator, slowly add 85kg fat alcohol polyethylene ether sodium sulfate, to dissolving fully; Keep 40～50 ℃ of temperature, under continuously stirring, add the 150kg Sodium dodecylbenzene sulfonate, to dissolving fully; Add the 40kg castor oil polyoxyethylene ether, to dissolving fully; Add the 45kg coconut acid diethanolamide, to dissolving fully; Be cooled to below 40 ℃, adding content is 95% industrial spirit 20kg, stirs; Regulate pH value to 7.0～7.5 (pH test paper methods) with dilute sulphuric acid, promptly become the emulsifying agent finished product.
2, the preparation of polyvinyl formal solution
In reactor, add industrial water purification 1000kg, be heated to 90～95 ℃, start agitator, slowly add polyvinyl alcohol 100kg, maintain the temperature at more than 90 ℃, to all dissolvings; Be cooled to about 70 ℃, add rare HCl and regulate pH value to 2.0; Add formaldehyde solution 40kg, reaction times 30～35min stops hot water circulation; Add aqueous solution of urea (25kg urea is mixed with aqueous solution of urea), with unnecessary formaldehyde reaction generation methylolurea; Regulate pH value to 7.0～7.5 (pH test paper methods) with the NaOH aqueous solution, promptly become polyvinyl formal solution.
3, polyacrylamide solution preparation
In reactor, add industrial water purification 500kg, be heated to 50 ℃～60 ℃ (being no more than 60 ℃), slowly add 10kg anion-polyacrylamide (molecular weight 400～6,000,000),, promptly become polyacrylamide solution to dissolving fully.
4, the preparation of nanometer-submicron level PVA mixed polymers
Polyvinyl formal solution 1000kg is mixed with polyacrylamide solution 500kg, start agitator, till mixing; Add the 100kg emulsifying agent again, stir and make its complete emulsification, promptly become polyvinyl formal-polyacrylamide mix emulsion fluid; This mix emulsion fluid is put into High shear device, and 20,000 r/min speed down cut 5min promptly become nanometer-submicron level PVA formal-polyacrylamide and mix the polymers aqueous solution, are called for short nanometer-submicron level PVA mixed polymers.
Claims (1)
1. the production method of a water-soluble nano-submicron level PVA mixed polymer as fertilizer cementing and coating agent, its feature is made up of following technological process:
(1) preparation of emulsifying agent: in reactor, add industrial water purification, be heated to 45 ℃～50 ℃, under agitation condition, slowly add quality 8%～10% fat alcohol polyethylene ether sodium sulfate, the dissolving back keeps 40 ℃～50 ℃ of temperature fully, under continuously stirring, add quality 15%～20% Sodium dodecylbenzene sulfonate successively, 4%～5% castor oil polyoxyethylene ether, 4%～5% coconut acid diethanolamide, add a kind of down after every kind of surfactant dissolves again, all be cooled to below 40 ℃ after the dissolving, add quality 2%～3% industrial spirit, mix, measure the pH value, regulate pH value to 7.0, promptly become the emulsifying agent finished product with dilute sulphuric acid;
(2) preparation polyvinyl formal solution: in reactor, add industrial water purification, be heated to 90 ℃～95 ℃, start agitator, slowly add quality 10%～15% polyvinyl alcohol, maintain the temperature at more than 90 ℃, all be cooled to about 70 ℃ after the dissolving, add dilute hydrochloric acid solution and regulate pH value to 2.0, add quality 4%～6%, content is 36%～37% formaldehyde solution, and reaction 30～35min stops hot water circulation, add 2%～3% aqueous solution of urea, generate methylolurea with unnecessary formaldehyde, regulate pH value to 7.0, promptly become polyvinyl formal solution with the NaOH aqueous solution;
(3) preparation polyacrylamide solution: in reactor, add industrial water purification, be heated to 50 ℃～60 ℃, slowly add the anion-polyacrylamide of quality 2%～2.5%, molecular weight 400～6,000,000, all promptly become polyacrylamide solution after the dissolving;
(4) prepare nanometer-submicron level PVA mixed polymers: polyvinyl formal solution is mixed by mass ratio with polyacrylamide solution at 2: 1, add mixing solutions quality 5%～10% mentioned emulsifier, stir and make its emulsification, put into High shear device of the present invention, 20,000 r/min speed down cuts, 5～10min, promptly become nanometer-submicron level PVA formal-polyacrylamide and mix the polymers aqueous solution, be called for short nanometer-submicron level PVA mixed polymers; More than employed High shear device by forming with lower member:
1) motor: Jiangsu star-wheel high-speed electric expreess locomotive device fabrication company makes;
2) cutter shaft and high-shear cutter: adopt the processing and manufacturing of high chrome high-nickel austenitic stainless steel material, shear knife is a spination, and cutter shaft is connected with motor output shaft by three-jaw chuck;
3) stainless steel tank body: diameter 500mm, high 700mm;
4) guide shell: in be lining in the effect that water conservancy diversion is played at tank body middle part, make material be turbulence state circulation high-shear, simplified diameter 200mm, high 350mm;
5) capping: the stainless steel cover periphery reaches and is coupling to touch partly and all is stained with sealing-ring, plays airtight effect,
6) feed inlet and outlet: opening for feed is positioned at tank body top, and discharge port is positioned at the tank body bottom.
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| CNB2004100913158A CN100554329C (en) | 2004-11-22 | 2004-11-22 | The nanometer-submicron level PVA mixed polymer as fertilizer cementing coating agent preparation method |
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| CN100554329C true CN100554329C (en) | 2009-10-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101486615B (en) * | 2009-02-23 | 2012-01-25 | 烟台五洲施得富肥料有限公司 | Preparation of fertilizer coating sustained-release agent |
| CN103396242A (en) * | 2013-08-08 | 2013-11-20 | 徐庆海 | Production process and device for organization of inorganic fertilizers |
| CN106748303A (en) * | 2017-02-20 | 2017-05-31 | 山东鲁北企业集团总公司 | A kind of chemical fertilizer controlled release agent and preparation method thereof |
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| CN1388169A (en) * | 2002-07-26 | 2003-01-01 | 张夫道 | Production process and application of nano-level coagulated material of waste plastic and starch |
| CN1414033A (en) * | 2002-08-09 | 2003-04-30 | 张夫道 | Production technology of nano-clay-polyester mixed polymer fertilizer coating cementing agent |
| CN1417173A (en) * | 2002-11-11 | 2003-05-14 | 张夫道 | Production techn of coating cement for nano sulfonated lignin mixture fertilizer |
| CN1470485A (en) * | 2002-07-23 | 2004-01-28 | 中国科学院南京土壤研究所 | Carrier type slow-release fertilizer and its preparing method |
| CN1506335A (en) * | 2002-12-11 | 2004-06-23 | 北京市农林科学院植物营养与资源研究 | Synthesis of urea-formaldehyde controlled releasing fertilizer |
| JP2004204038A (en) * | 2002-12-25 | 2004-07-22 | Mitsui Chemicals Inc | Biodegradable water dispersion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470485A (en) * | 2002-07-23 | 2004-01-28 | 中国科学院南京土壤研究所 | Carrier type slow-release fertilizer and its preparing method |
| CN1388169A (en) * | 2002-07-26 | 2003-01-01 | 张夫道 | Production process and application of nano-level coagulated material of waste plastic and starch |
| CN1414033A (en) * | 2002-08-09 | 2003-04-30 | 张夫道 | Production technology of nano-clay-polyester mixed polymer fertilizer coating cementing agent |
| CN1417173A (en) * | 2002-11-11 | 2003-05-14 | 张夫道 | Production techn of coating cement for nano sulfonated lignin mixture fertilizer |
| CN1506335A (en) * | 2002-12-11 | 2004-06-23 | 北京市农林科学院植物营养与资源研究 | Synthesis of urea-formaldehyde controlled releasing fertilizer |
| JP2004204038A (en) * | 2002-12-25 | 2004-07-22 | Mitsui Chemicals Inc | Biodegradable water dispersion |
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