CN106046234A - Preparation method for novel ion-type vinyl acetate emulsion used for combating desertification of highly saline-alkaline soil - Google Patents
Preparation method for novel ion-type vinyl acetate emulsion used for combating desertification of highly saline-alkaline soil Download PDFInfo
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Abstract
The invention relates to a preparation method for a novel ion-type vinyl acetate emulsion used for combating desertification of highly saline-alkaline soil. The method comprises the following steps: carrying out copolymerization on vinyl acetate used as main monomer, dibutyl maleate used as soft monomer, acrylic acid used as auxiliary monomer and sulfonic acid group-containing monomer used as functional monomer through seeded emulsion polymerization; and synthesizing the saline-alkaline-resistant polyvinyl acetate copolymerized emulsion with a water-soluble peroxide compound as an initiator and anionic and non-ionic emulsifiers as composite emulsification system. When applied to highly saline-alkaline sand, the prepared novel ion-type vinyl acetate emulsion has excellent bonding performance and wind erosion resistance and does not pollute environment nor influence plant growth; the preparation method is simple and suitable for large-scale production; and the novel ion-type vinyl acetate emulsion is applicable to prevention and treatment of desertification of highly saline-alkaline sand.
Description
Technical field
Present invention relates particularly to a kind of novel ionic vinyl acetate emulsion preparation method for high salinity ground desert treatment, belong to field of chemical sand fixation.
Background technology
Salt-soda soil desertification is just annoying the world today as extremely important environment and social problem, threatens the survival and development of the mankind, and countries in the world are all using containing that salt-soda soil desertification is as improvement of the ecological environment and the important topic of sustainable development.
China's salt-soda soil area is about 9913 × 104hm2, wherein modern salt-soda soil about 3.693 × 107hm2, remaining salt-soda soil about 4.487 × 107hm2, and still have 1.733 × 107hm2Potential salinized soil, be mainly distributed on the Plain of 23 provinces, municipalities and autonomous regions of national 5 great Qu, including coastal saline-alkali Tu Qu, Huang-Huai-Hai plain saline-alkali soil district, semiarid saline-alkali soil district, northwest and arid saline-alkali soil district and saline-alkali soil district, northeast.Therefore, administer and improve salt-soda soil Desertification and have become as China's developing agricultural, the vital task of improve the ecological environment, promote economy and Ecological Sustainable Development.
Abroad for the research relatively morning in salt-soda soil, the scholar of the states such as the U.S., the former Soviet Union, Australia, Israel, Japan began to study the salinization of soil in the thirties in 20th century.Whether the former Russian scholar once just used artificial drainage to launch heated argument to the problem preventing and treating Pedotransfer function: the scholar represented with B.A. Sa Wu Mianwei thinks that the major measure of preventing and treating should be control water and learotation system, and the scholar using B.A. Ke Fuda as representative then advises the Main Means building drainage network as preventing and treating.Additionally, the scientist of the states such as Pakistan, India, Egypt, Israel and Australia has carried out substantial amounts of research in terms of plant, to improve the Salt And Alkali Tolerance adaptation ability of plant.
Salt-soda soil is researched and developed control and is started from the 1950's by China on a large scale, uses the single measures such as water conservancy, agricultural, physics, chemistry to improve more.The mid-1960s, Bears is firm et al. advocate under, utilize irrigation and drainage by well to obtain good effect.Although these hydraulic engineering measures lowering of watertable, prevent and treat the salinization of soil in terms of play a role.It is but irrigate to rinse and need freshwater resources and great amount of investment with draining, and the biggest for the cost of maintenance and management, it is most important that, these measures the most fundamentally solve salt-soda soil Desertification.
For a long time, chemical sand fixing material is being used to carry out in the practice of high salinity ground desert treatment, the problem that always there is sand fixation material Salt And Alkali Tolerance poor performance.Up to now, also there is no effective material high salinity ground desertification can administered.The polyurethane sand-consolidating agent that toray company develops, though being successfully applied to the fixation experiment in the multiple area of China, but the saline and alkaline desert area in Qinghai, fails the effect obtained always.In the face of China's salt-soda soil desertification area still in the severe situation expanded, it is developed to effectively contain the suitable material of high salinity ground desertification, is a challenge the most urgent.
Summary of the invention
The subject matter existed for current sand fixation material, it is an object of the invention to provide the preparation method of a kind of novel ionic vinyl acetate emulsion for high salinity ground desert treatment, solve existing sand fixation material in problems such as the easily efflorescence of high salinity ground, consolidation strength differences.The emulsion sand fixation material using this method to prepare, has the features such as good Saline alkali tolerance, stability, caking property, and production cost is low, and preparation technology is simple.
To achieve these goals, the technology path that the present invention uses is as follows: the preparation method of a kind of novel ionic vinyl acetate emulsion for high salinity ground desert treatment, includes three below step.
1) mixed dissolution
10～50 parts of vinylacetates, 0.5～5 part of acrylic acid and 1～20 part of dibutyl maleate comonomer are carried out premixing and obtain mix monomer；Being dissolved in 10～40 parts of deionized waters by 0.2～2 part of initiator, 1～5 part is dissolved in 10～40 parts of deionized waters containing sulfonic function monomer；
2) pre-emulsification
30～70 parts of deionized waters and whole blended emulsifiers is added in reactor, it is heated to 50～60 DEG C, after reaction 15～60min, continues to be heated to 60～70 DEG C, add 1/4～1/3 (mass fraction of shared initiator gross weight) initiator, emulsifying 10～60min；
3) polymerization
Above-mentioned mixed liquor is warming up to 70～85 DEG C, add 1/5～1/3 (mass fraction of shared mix monomer gross weight) vinylacetate, the mix monomer of acrylic acid and dibutyl maleate comonomer and 1/5～1/3 (mass fraction of shared sulfonic group total weight of monomer) monomer solution Han sulfonic group, after initiation reaction 10～45min, it is slowly added dropwise remaining initiator and residual monomer with constant pressure funnel, initiator and mix monomer is kept Tong Bu to drip off, emulsion polymerization 3.0～6.0h, 85～95 DEG C it are warming up to after reaction, insulation 1.0～3.0h, it is cooled to room temperature, discharging, obtain Salt And Alkali Tolerance and fix the sand emulsion.
By such scheme, described blended emulsifier is the compound system of anionic and nonionic emulsifier.Wherein, in complex emulsifier, anionic emulsifier and nonionic emulsifier mass ratio are 1: 5～5: 1；Anionic emulsifier is any one or more in sodium lauryl sulphate, dodecylbenzene sodium sulfonate, triethanolamine sodium sulfonate, enuatrol, Monododecylphosphate potassium, AESA etc.；Nonionic emulsifier is any one or more in octyl phenol polyoxyethylene alcohol, nonylphenol polyethylene oxide ether, polyethers L35, polyethers L45, polyethers F68, polysorbas20, polysorbate60, Tween 80, Span 65, Span 80.
By such scheme, described containing sulfonic group function monomer be methylpropene sodium sulfonate, Sodium styrene sulfonate, 2-acrylamide-2-methylpro panesulfonic acid, to one or more in sodium vinyl sulfonate, acrylic sodium sulfonate monomer.
By such scheme, described initiator is water miscible potassium peroxydisulfate, Ammonium persulfate., H2O2In any one.
The present invention is as follows for the action principle of high salinity desert treatment:
Chemical sand-fixing mechanism: vinyl acetate emulsion has adhesive property, although being closely to pile up together between the grains of sand, but there are still small passage (more than 8 μm), once this emulsion is sprayed onto sandy land surface, just penetrate into husky internal less than the drop of 8 μm, cemented together with the grains of sand, then form skinning at sandy land surface more than the drop of 8 μm, after it solidifies, sand ground is fixed.In addition to the bonding effect of vinyl acetate emulsion, there is also the factor of fixing the sand of some complexity, if this emulsion particle surface is with electric charge, can be by electric charge interphase interaction between they and the grains of sand, affect " attract-repel " power between the adjacently situated surfaces grains of sand, simultaneously contained in this emulsion molecule functional group can produce intramolecular effect, forms continuously or discontinuously network structure, is securely bonded together by the grains of sand.
Salt And Alkali Tolerance mechanism: containing the strong hydrability anionic group insensitive to salt in vinyl acetate copolymer emulsion molecule, such as sulfonic acid group.Work as Na+、Ca2+、Mg2+In the presence of ion, sulfonic dense ionization effect increases the hydrodynamic volume of macromolecular chain, and emulsion apparent viscosity is basically unchanged, and emulsion will show good Salt And Alkali Tolerance performance.
Simultaneously, the most also need to introduce the bigger side base of volume to improve macromole chain rigidity, make the curling difficulty of this emulsion strand, the mechanics radius that strand rotates increases, the violent decline of the macromole coil dimension that inorganic electrolyte causes is added, so that the Salt And Alkali Tolerance ability of emulsion is improved with suppression.
The invention have the advantages that and beneficial effect:
(1) with wide material sources, cheap vinylacetate as main monomer, it is greatly reduced and fixes the sand cost.
(2) addition of functional monomer, drastically increases the Salt And Alkali Tolerance performance of emulsion, uses it for the improvement of high salinity desertification, alleviates salt-soda soil desertification area still in the severe situation expanded rapidly.
(3) bonding course can effectively suppress the evaporation of bottom moisture, strengthens water-retaining property, can combine with plantation saline alkali tolerant plant, improve sand-fixing effect, accelerate the ecological recovery on ground, high salinity desert.
Accompanying drawing explanation
Fig. 1 is vinyl acetate emulsion concentration and comprcssive strength relation curve in the embodiment of the present invention 1
Fig. 2 is the comprcssive strength of vinyl acetate emulsion and the relation curve of freeze thawing time in the embodiment of the present invention 1
Fig. 3 is the comprcssive strength of vinyl acetate emulsion and the relation curve of thermal aging time in the embodiment of the present invention 1
Fig. 4 is the impact that in the embodiment of the present invention 1, plant (little caragana) is grown by vinyl acetate emulsion, uses and fixes the sand emulsion and not using and fix the sand the growing state of plant after emulsion.
Detailed description of the invention
In order to be better understood from the present invention; the following examples are to further illustrate the present invention; be necessary it is pointed out here that be; following example are served only for that the invention will be further described; it is not intended that limiting the scope of the invention; the present invention is made some nonessential improvement and adjustment according to the invention described above content by the person skilled in the art in this field, still falls within scope.
Embodiment 1
1.0 parts of acrylic acid of 32.5 parts of vinylacetates and 16.5 parts of dibutyl maleate monomers are carried out premixing and obtain mix monomer.Being dissolved in 30 parts of deionized waters by 0.3 part of potassium peroxydisulfate, 1.2 parts of Sodium styrene sulfonate are dissolved in 30 parts of water.null60 parts of water are added in reactor、0.67 part of sodium lauryl sulphate and 1.5 parts of L35，It is heated to 50 DEG C，After reaction 15min，Continue to be heated to 65 DEG C，Add 1/3 (mass fraction of shared potassium peroxydisulfate gross weight) potassium persulfate solution，Emulsifying 20 minutes，Then heat to 74 DEG C，(mass fraction of the shared mix monomer gross weight) vinylacetate that adds 1/3、The mix monomer of acrylic acid and dibutyl maleate and 1/3 (mass fraction of shared Sodium styrene sulfonate gross weight) styrene sulfonic acid sodium water solution，After reaction 30min，It is slowly added dropwise remaining initiator with constant pressure funnel，It is slowly added dropwise residual monomer simultaneously，Initiator and all monomers are kept Tong Bu to drip off，Time for adding is 4.0h，85 DEG C it are warming up to after being added dropwise to complete，Insulation 1.0h，Then room temperature it is down to，Discharging，Obtain salt tolerant alkaline and fix the sand emulsion.
The preparation of Sha Mo: the salt tolerant alkaline of preparation fixes the sand emulsion is made into the diluent that solid content is 2%, 3%, 4%, 6%, 8%, 10%；Weigh the sandy soil diluent above-mentioned with 1.0g that 10g salinity is 3% and mix homogeneously the husky mould of preparation (a diameter of 2.0cm, height is 2.2cm), 80 DEG C of dry 2h, i.e. get Sha Mo.
The freeze-thaw stability of vinyl acetate emulsion measures: above-mentioned prepared husky mould is put into freezing 22h in the environment of-18 DEG C, then puts sand mould to delay at room temperature and freezes 2h, is designated as a cycle period, measures the comprcssive strength situation of change in its 10 cycles.
The heat aging performance of vinyl acetate emulsion measures: above-mentioned prepared husky mould is put into 24h in the baking oven of 60 DEG C, is a cycle period, measures the comprcssive strength situation of change in its 10 cycles.
Fig. 1 is the comprcssive strength of different solid content vinyl acetate emulsion, the emulsion of fixing the sand adding functional monomer is experimental group, and the emulsion of fixing the sand not adding functional monomer is matched group, as can be seen from the figure, the addition of functional monomer drastically increases the comprcssive strength of high salinity Burmannia coelestis D. Don. mould, comprcssive strength means that greatly bonding course is not susceptible to external force and destroys, and shows that this emulsion has preferable saline-alkali tolerance, is able to take the change of desert Environment external force.
Fig. 2 is the freeze-thaw stability of vinyl acetate emulsion, it can be seen that along with the increase of freezing and thawing cycle, the comprcssive strength of Sha Mo is not changed in substantially, shows that this emulsion has good freeze thawing resistance stability, is able to take the change of desert Environment temperature.
Fig. 3 is the thermal ageing resistant performance of vinyl acetate emulsion, it can be seen that along with the increase in heat ageing cycle, the comprcssive strength of Sha Mo is not changed in substantially, shows that this emulsion has good resistance to heat aging, is able to take the change of desert Environment temperature.And then provide feasibility for this emulsion in the use of high salinity sand ground.
Fig. 4 is the impact that plant (little caragana) is grown by vinyl acetate emulsion, and left figure is to spray plant growing situation after this emulsion, and right figure is matched group test.It can be seen that plant all can be grown after spraying this emulsion smoothly, have substantially no effect on the bud ratio of plant, and growing way is significantly better than the plant growing situation without this emulsion.
Embodiment 2
30 parts of vinylacetates, 2 parts of acrylic acid and 15 parts of dibutyl maleate monomers are carried out premixing and obtain mix monomer.Being dissolved in 15 parts of deionized waters by 1.0 parts of potassium peroxydisulfates, 2.0 part of 2. acrylamido .2. methyl propane sulfonic acid is dissolved in 20 parts of water.null70 parts of water are added in reactor、1.0 parts of sodium lauryl sulphates and 2.0 parts of polysorbate60s，It is heated to 55 DEG C，After reaction 30min，Continue to be heated to 65 DEG C，Add 1/3 (mass fraction of shared potassium peroxydisulfate gross weight) potassium persulfate solution，Emulsifying 30 minutes，Then heat to 75 DEG C，The mix monomer of (mass fraction of the shared mix monomer gross weight) vinylacetate that adds 1/5 and dibutyl maleate and 1/3 (mass fraction of shared 2-acrylamide-2-methylpro panesulfonic acid gross weight) 2-acrylamide-2-methylpro panesulfonic acid aqueous solution，Initiation reaction 10min，It is slowly added dropwise remaining initiator with constant pressure funnel，It is slowly added dropwise residual monomer simultaneously，Initiator and all monomers are kept Tong Bu to drip off，Time for adding is 4.0h，90 DEG C it are warming up to after being added dropwise to complete，Insulation 1.0h，Then room temperature it is down to，Discharging，Obtain salt tolerant alkaline and fix the sand emulsion.
Embodiment 3
50 parts of vinylacetates, 1.5 parts of acrylic acid and 10 parts of dibutyl maleate monomers are carried out premixing and obtain mix monomer.Being dissolved in 20 parts of deionized waters by 1.5 parts of potassium peroxydisulfates, sodium vinyl sulfonate is dissolved in 20 parts of water by 2.0 parts.null30 parts of water are added in reactor、1.0 parts of enuatrols and 2.0 parts of polyethers L35，It is heated to 55 DEG C，After reaction 20min，Continue to be heated to 65 DEG C，Add 1/4 (mass fraction of shared potassium peroxydisulfate gross weight) potassium persulfate solution，Emulsifying 30 minutes，Then heat to 75 DEG C，The mix monomer of (mass fraction of the shared mix monomer gross weight) vinylacetate that adds 1/4 and dibutyl maleate and 1/5 (the shared mass fraction to sodium vinyl sulfonate gross weight) are to sodium vinylsulphonate solution，Initiation reaction 10min，It is slowly added dropwise remaining initiator with constant pressure funnel，It is slowly added dropwise residual monomer simultaneously，Initiator and all monomers are kept Tong Bu to drip off，Time for adding is 4.0h，90 DEG C it are warming up to after being added dropwise to complete，Insulation 1.0h，Then room temperature it is down to，Discharging，Obtain salt tolerant alkaline and fix the sand emulsion.
Embodiment 4
35 parts of vinylacetates, 2.4 parts of acrylic acid and 15 parts of dibutyl maleate monomers are carried out premixing and obtain mix monomer.Being dissolved in 25 parts of deionized waters by 1.6 parts of Ammonium persulfate .s, 4.0 parts of acrylic sodium sulfonates are dissolved in 20 parts of water.null50 parts of water are added in reactor、1.6 parts of dodecylbenzene sodium sulfonate and 1.4 parts of octyl phenol polyoxy ether，It is heated to 58 DEG C，After reaction 30min，Continue to be heated to 62 DEG C，Add 1/3 (mass fraction of shared Ammonium persulfate. gross weight) ammonium persulfate solution，Emulsifying 30 minutes，Then heat to 72 DEG C，The mix monomer of (mass fraction of the shared mix monomer gross weight) vinylacetate that adds 1/5 and dibutyl maleate and 1/3 (mass fraction of shared acrylic sodium sulfonate gross weight) acrylic sodium sulfonate aqueous solution，Initiation reaction 10min，It is slowly added dropwise remaining initiator with constant pressure funnel，It is slowly added dropwise residual monomer simultaneously，Initiator and all monomers are kept Tong Bu to drip off，Time for adding is 3.0h，88 DEG C it are warming up to after being added dropwise to complete，Insulation 1.0h，Then room temperature it is down to，Discharging，Obtain salt tolerant alkaline and fix the sand emulsion.
Embodiment 5
40 parts of vinylacetates, 3 parts of acrylic acid and 10 parts of dibutyl maleate monomers are carried out premixing and obtain mix monomer.Being dissolved in 25 parts of deionized waters by 1.2 parts of Ammonium persulfate .s, 3.5 parts of methylpropene sodium sulfonates are dissolved in 20 parts of water.null40 parts of water are added in reactor、1.7 parts of sodium lauryl sulphates and 1.7 parts of polyethers L45，It is heated to 55 DEG C，After reaction 30min，Continue to be heated to 65 DEG C，Add 1/3 (mass fraction of shared Ammonium persulfate. gross weight) ammonium persulfate solution，Emulsifying 20 minutes，Then heat to 72 DEG C，The mix monomer of (mass fraction of the shared mix monomer gross weight) vinylacetate that adds 1/4 and dibutyl maleate and 1/3 (mass fraction of shared methylpropene sodium sulfonate gross weight) methylpropene sodium sulfonate aqueous solution，Initiation reaction 15min，It is slowly added dropwise remaining initiator with constant pressure funnel，It is slowly added dropwise residual monomer simultaneously，Initiator and all monomers are kept Tong Bu to drip off，Time for adding is 4.0h，88 DEG C it are warming up to after being added dropwise to complete，Insulation 1.0h，Then room temperature it is down to，Discharging，Obtain salt tolerant alkaline and fix the sand emulsion.
Claims (4)
1. for a novel ionic vinyl acetate emulsion preparation method for high salinity ground desert treatment, its feature
Be to comprise the steps: based on the number of quality shared by each raw material, this emulsion be by deionized water 50～150 parts,
Compound emulsifying agent 1～5 parts, vinylacetate 10～50 parts, dibutyl maleate 1～20 parts, containing sulfonic group single group
Body 1～5 parts, acrylic acid 0.5～5 parts and initiator 0.2～2 parts；It it is 50～95 DEG C and response time in test temperature
Under conditions of being 4～15h, prepare through seeded emulsion polymerization copolyreaction；Its emulsion preparation technology include mixed dissolution,
Pre-emulsification, polymerization,
1) mixed dissolution
10～50 parts of vinylacetates, 0.5～5 part of acrylic acid and 1～20 part of dibutyl maleate comonomer are entered
Row premixing obtains mix monomer；Being dissolved in 10～40 parts of deionized waters by 0.2～2 part of initiator, 1～5 part contains
Sulfonic function monomer is dissolved in 10～40 parts of deionized waters；
2) pre-emulsification
In reactor, add 30～70 parts of deionized waters and whole blended emulsifiers, be heated to 50～60 DEG C,
After reaction 15～60min, continue to be heated to 60～70 DEG C, add the 1/4～1/3 (matter of shared initiator gross weight
Amount mark) initiator, emulsifying 10～60min；
3) polymerization
Above-mentioned mixed liquor is warming up to 70～85 DEG C, adds 1/5～1/3 (mass fraction of shared mix monomer gross weight)
The mix monomer of vinylacetate, acrylic acid and dibutyl maleate and 1/5～1/3 (shared sulfonic group total weight of monomer
Mass fraction) monomer solution Han sulfonic group, after initiation reaction 10～45min, it is slowly added dropwise with constant pressure funnel
Remaining initiator and residual monomer, keep initiator and mix monomer Tong Bu to drip off, emulsion polymerization 3.0～6.0h,
It is warming up to 85～95 DEG C after reaction, is incubated 1.0～3.0h, is cooled to room temperature, discharging, obtain Salt And Alkali Tolerance and fix the sand emulsion.
A kind of novel ionic vinyl acetate for high salinity ground desert treatment the most according to claim 1
Ester emulsion preparation method, it is characterised in that this blended emulsifier is the complex of anionic and nonionic emulsifier
System；Wherein, in complex emulsifier, anionic emulsifier and nonionic emulsifier mass ratio are 1: 5～5: 1；
Anionic emulsifier be sodium lauryl sulphate, dodecylbenzene sodium sulfonate, triethanolamine sodium sulfonate, enuatrol,
Any one or more in Monododecylphosphate potassium, AESA；Nonionic breast
Agent is octyl phenol polyoxyethylene alcohol, nonylphenol polyethylene oxide ether, polyethers L35, polyethers L45, polyethers F68, tween
20, any one or more in polysorbate60, Tween 80, Span 65, Span 80.
A kind of novel ionic vinyl acetate for high salinity ground desert treatment the most according to claim 1
Ester emulsion preparation method, it is characterised in that containing sulfonic group function monomer be methylpropene sodium sulfonate, Sodium styrene sulfonate,
2-acrylamide-2-methylpro panesulfonic acid, to one or more in sodium vinyl sulfonate, acrylic sodium sulfonate monomer.
A kind of novel ionic vinyl acetate for high salinity ground desert treatment the most according to claim 1
Ester emulsion preparation method, it is characterised in that this initiator is water miscible potassium peroxydisulfate, Ammonium persulfate., H2O2In appoint
A kind of.
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| CN112831294A (en) * | 2021-01-29 | 2021-05-25 | 上海应用技术大学 | Re-wettable water-based adhesive, preparation method and application |
| CN113105577A (en) * | 2021-03-23 | 2021-07-13 | 商洛学院 | Repairing agent for heavy metal pollution control and ecological restoration and preparation method thereof |
| CN114015390A (en) * | 2021-12-08 | 2022-02-08 | 崔俊 | Water-based EVA adhesive and preparation method thereof |
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