CN103723688B - A kind ofly improve the inorganic oxidant of encapsulation rate or the method for modifying of inorganic salt - Google Patents
A kind ofly improve the inorganic oxidant of encapsulation rate or the method for modifying of inorganic salt Download PDFInfo
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Abstract
Improve the inorganic oxidant of encapsulation rate or a method of modifying for inorganic salt, belong to novel material, technical field of chemistry and chemical engineering, particularly the production technology of microcapsule.Drip the vitriol oil after first aluminum chloride being dissolved in deionized water, add methyl alcohol, propyl carbinol and 1,2-PD after intensification, temperature rising reflux reaction, to terminating solid phase washing that rear negate should produce, dry, obtains product; Basic zirconium chloride, ethanol, stearic acid and acrylic acid mixture post-heating are carried out back flow reaction, adds step again and obtain product after reaction terminates, continue back flow reaction, reaction terminates solid phase washing that rear negate should produce, dry, obtains product; Inorganic oxidant or inorganic salt and upper step product are reacted under agitation, obtains the modifier of inorganic oxidant or inorganic salt.By above technique, modifier surface has connected the chain of oleophilic drainage, can improve the encapsulation ratio of inorganic oxidant or inorganic salt microcapsule.
Description
Technical field
The invention belongs to novel material, technical field of chemistry and chemical engineering, particularly the production technology of microcapsule.
Background technology
Microcapsulary utilizes natural or synthesized polymer material as lapping, solid particulate, liquid or gas had a kind of minigel technology of semipermeability or sealing cyst membrane as the coated formation of core material.The 1950's, microcapsulary is applied to transfer paper preparation by the U.S. first, opens new era of microcapsulary.To 20 century 70s, Japan develops release drug microcapsule, latent crosslinker microcapsule etc.After this there is numerous microencapsulated products and technique, and made microcapsulary be widely used in multiple fields such as pharmaceutical industry, coating, sizing agent, food, fire retardant, petrochemical complex, ink and weaving.
The inorganic oxidant such as cerium oxide, sodium peroxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate or inorganic salt all belong to wetting ability, the conventional initiator doing the product such as latex or polymerizable acrylic monomer liquid, vinyl acetate between to for plastic, vinylchlorid is also the initiator etc. of vinylbenzene, vinyl cyanide, divinyl isocolloid generation interpolymerization simultaneously.Slowly can be polymerized at a certain temperature to realize above-mentioned monomer, preparing the polymkeric substance that molecular weight is higher or lower.Current people are by technology such as pressed disc method, fluidized bed process, spray-drying process, situ aggregation methods, above-mentioned inorganic oxidant or inorganic salt being prepared into can the microcapsule of Co ntrolled release, realize monomer can slowly be polymerized at a certain temperature, prepare the polymkeric substance that molecular weight is higher or lower.But, because above-mentioned conventional inorganic oxidant or inorganic salt surface are in smooth form, so be difficult to effectively macromolecular material that is natural or synthesis be deposited or be coated on its surface, form complete core-shell structure microcapsule.This reduces encapsulation ratio and the qualification rate of microcapsule product to a great extent.
Summary of the invention
The present invention seeks to carry and a kind ofly can improve the inorganic oxidant of the encapsulation ratio of microcapsule product or the modifier working method of inorganic salt.
The present invention includes following steps:
1) vitriol oil is dripped after aluminum chloride being dissolved in deionized water, add methyl alcohol, propyl carbinol and 1,2-PD after system being warming up to 40 DEG C, system is increased to 60 DEG C and carries out back flow reaction, reaction terminates solid phase washing that rear negate should produce, dry, obtains product;
2) basic zirconium chloride, ethanol, stearic acid and acrylic acid mixture post-heating are carried out back flow reaction, add step 1) again and obtain product after reaction terminates, continue back flow reaction, reaction terminates solid phase washing that rear negate should produce, dry, obtains product;
3) by inorganic oxidant or inorganic salt and step 2) product reacts under agitation, obtains the modifier of inorganic oxidant or inorganic salt.
The chain of oleophilic drainage has been connected by the inorganic oxidant of above technique or the modifier surface of inorganic salt, thus reduce inorganic oxidant or the interfacial tension between inorganic salt and macromolecular material, in follow-up packing technology, macromolecular material is easy to deposition or is coated on inorganic oxidant or inorganic salt surface, thus improves the encapsulation ratio of inorganic oxidant or inorganic salt microcapsule.
Described aluminum chloride, deionized water, the vitriol oil, methyl alcohol, propyl carbinol, 1,2-PD, basic zirconium chloride, ethanol, stearic acid, vinylformic acid and inorganic oxidant or inorganic salt account for 3% ~ 5%, 2% ~ 4%, 0.5% ~ 1.5%, 3% ~ 8%, 0.5% ~ 2%, 0.5% ~ 1.5%, 0.5% ~ 2%, 2% ~ 5%, 0.5% ~ 1%, 1% ~ 3% and 67% ~ 86% of the total mass that feeds intake respectively.Optimum inorganic oxidant or the finishing effect of inorganic salt can be obtained at the feed ratio of above-mentioned each raw material.
Inorganic oxidant or inorganic salt are any one in sodium peroxide, cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of sodium peroxide before modified.
Fig. 2 is the scanning electron microscope (SEM) photograph of the sodium peroxide adopting present invention process modified.
Fig. 3 is the scanning electron microscope (SEM) photograph will obtained after sodium peroxide deposition polyacrylonitrile before modified.
Fig. 4 is the scanning electron microscope (SEM) photograph will obtained after modified sodium peroxide deposition polyacrylonitrile.
Embodiment
One, modified technique:
(1) aluminum chloride and the deionized water of getting respective quality ratio add in the there-necked flask of band stirring and reflux, are stirred to and dissolve completely, then slowly instill the quantitative vitriol oil.Said apparatus temperature of reaction is increased to 40 DEG C, adds the mixed solution of the methyl alcohol of respective quality ratio, propyl carbinol and 1,2-PD, continue raised temperature to 60 DEG C, heating reflux reaction 2 hours.Stopped reaction, product obtains product 1 after the process of washing and dry.
(2) get the basic zirconium chloride of respective quality ratio, ethanol, stearic acid and acrylic acid mixture in there-necked flask, heating reflux reaction, after 2 hours, adds above-mentioned product 1, and makes it continue to react 2 hours under reflux.Stopped reaction device, sample, after the process of washing and drying, obtains product 2.
(3) a certain amount of sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.) is got in there-necked flask, under the condition stirred, slowly add above-mentioned product 2, and improve stirring velocity to 1000 rev/min, react after 30 minutes, namely obtain modified sodium peroxide product.
The per-cent (100%) that concrete each component accounts for the gross weight that feeds intake is:
Scheme 1: aluminum chloride 3.5%, deionized water 2.8%, the vitriol oil 0.9%, methyl alcohol 5%, propyl carbinol 0.5%, 1,2-propylene glycol 0.7%, basic zirconium chloride 0.7%, ethanol 3%, stearic acid 0.5%, vinylformic acid 1%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).
Scheme 2: aluminum chloride 4%, deionized water 3%, the vitriol oil 1%, methyl alcohol 5.5%, propyl carbinol 0.8%, 1,2-propylene glycol 1%, basic zirconium chloride 1%, ethanol 4%, stearic acid 0.5%, vinylformic acid 1.5%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).
Scheme 3: aluminum chloride 4.5%, deionized water 3.5%, the vitriol oil 1.2%, methyl alcohol 8%, propyl carbinol 1%, 1,2-propylene glycol 1.5%, basic zirconium chloride 1.5%, ethanol 5%, stearic acid 1%, vinylformic acid 2%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).
Scheme 4: aluminum chloride 3%, deionized water 2.5%, the vitriol oil 0.7%, methyl alcohol 4%, propyl carbinol 1%, 1,2-propylene glycol 0.5%, basic zirconium chloride 0.5%, ethanol 3%, stearic acid 0.5%, vinylformic acid 0.8%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).
Scheme 5: aluminum chloride 5%, deionized water 3%, the vitriol oil 1.5%, methyl alcohol 7%, propyl carbinol 2%, 1,2-propylene glycol 1.5%, basic zirconium chloride 1.5%, ethanol 5%, stearic acid 1%, vinylformic acid 2%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).Scheme 6: aluminum chloride 3%, deionized water 2%, the vitriol oil 0.5%, methyl alcohol 4%, propyl carbinol 0.5%, 1,2-propylene glycol 0.5%, basic zirconium chloride 0.5%, ethanol 2%, stearic acid 0.5%, vinylformic acid 1%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).Scheme 7: aluminum chloride 5%, deionized water 4%, the vitriol oil 1.5%, methyl alcohol 8%, propyl carbinol 2%, 1,2-propylene glycol 1.5%, basic zirconium chloride 2%, ethanol 5%, stearic acid 1%, vinylformic acid 3%, all the other are sodium peroxide (or cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate etc.).
Two, product performance qualification:
Sodium peroxide forward and backward for modification is carried out scanning electron microscope result as shown in Figure 1, 2 respectively, sodium peroxide smooth surface before modified, and modified sodium peroxide is owing to connecting oleophilic drainage chain, the phenomenon that its surface presentation is coarse, can predict, be easy to deposit macromolecular material with modified sodium peroxide.
Three, apply:
Sodium peroxide forward and backward for modification is deposited respectively polyacrylonitrile laggard line scanning Electronic Speculum result as shown in Figure 3,4, the amount of sodium peroxide surface polyacrylonitrile deposition is little before modified, and the amount of the polyacrylonitrile of modified sodium peroxide surface deposition will improve a lot relatively before modified, and most of Sodium Persulfate surface is covered with polyacrylonitrile.
Claims (1)
1. improve the inorganic oxidant of encapsulation rate or a method of modifying for inorganic salt, it is characterized in that comprising the following steps:
1) vitriol oil is dripped after aluminum chloride being dissolved in deionized water, add methyl alcohol, propyl carbinol and 1,2-PD after system being warming up to 40 DEG C, system is increased to 60 DEG C and carries out back flow reaction, reaction terminates solid phase washing that rear negate should produce, dry, obtains product;
2) basic zirconium chloride, ethanol, stearic acid and acrylic acid mixture post-heating are carried out back flow reaction, add step 1) again and obtain product after reaction terminates, continue back flow reaction, reaction terminates solid phase washing that rear negate should produce, dry, obtains product;
3) by inorganic oxidant or inorganic salt and step 2) product reacts under agitation, obtains the modifier of inorganic oxidant or inorganic salt;
Described inorganic oxidant or inorganic salt are any one in sodium peroxide, cerium oxide, Sodium Persulfate, ammonium persulphate, Potassium Persulphate; Described aluminum chloride, deionized water, the vitriol oil, methyl alcohol, propyl carbinol, 1,2-PD, basic zirconium chloride, ethanol, stearic acid, vinylformic acid and inorganic oxidant or inorganic salt account for 3% ~ 5%, 2% ~ 4%, 0.5% ~ 1.5%, 3% ~ 8%, 0.5% ~ 2%, 0.5% ~ 1.5%, 0.5% ~ 2%, 2% ~ 5%, 0.5% ~ 1%, 1% ~ 3% and 67% ~ 86% of the total mass that feeds intake respectively.
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| CN104961102B (en) * | 2015-06-10 | 2017-04-12 | 贵州润晋碳元素材料有限公司 | Calcium peroxide moisture and water proofing treatment method |
| CN112934919B (en) * | 2021-02-05 | 2022-07-01 | 云南大地丰源环保有限公司 | Method for treating waste anhydrous aluminum chloride |
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| CN101775188A (en) * | 2009-12-30 | 2010-07-14 | 浙江工贸职业技术学院 | Method for preparing filling leather fatliquoring agent |
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| CN101775188A (en) * | 2009-12-30 | 2010-07-14 | 浙江工贸职业技术学院 | Method for preparing filling leather fatliquoring agent |
Non-Patent Citations (2)
| Title |
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| 氢氧化镁表面改性及其性能研究;闫海妮;《中国优秀硕士学位论文全文数据工程科技I辑》;20111231;第11-12、22-24页 * |
| 纳米氧化锌的改性及其对丙烯酸聚氨酯涂料的性能影响;张海凤;《中国优秀硕士学位论文全文数据工程科技I辑》;20101231;第20-30页 * |
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