CN103265046B - Serine/kaolinite intercalation complex prepared with 1.0nm hydrated kaolinite serving as intercalation precursor and preparation method - Google Patents
Serine/kaolinite intercalation complex prepared with 1.0nm hydrated kaolinite serving as intercalation precursor and preparation method Download PDFInfo
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Abstract
The invention discloses a serine/kaolinite intercalation complex prepared with 1.0nm hydrated kaolinite serving as an intercalation precursor and a preparation method. The preparation method comprises the following steps of: mixing hydrated kaolinite with interlamellar spacing of d001=1.0nm with serine solution; controlling the system to stir for a few minutes at relatively low temperature; and controlling to react for a few minutes at relatively high temperature, thus obtaining the serine/kaolinite intercalation complex. The spacing d001 of kaolinite layers expandes from 1.0nm before intercalating the serine to 1.14nm after intercalating the serine, the intercalating rate is up to 90 to 100%; the serine is arranged as a singe layer between the kaolinite layers in a way of being parallel to a kaolinite lamella; a carboxyl of the serine forms a hydrogen bond together with a hydroxyl on the inner surface of the kaolinite, and an amidogen forms another hydrogen bond together with an oxygen atom of a kaolinite silica layer. The preparation method is simple in preparation process and realizes batch production, and the prepared serine/kaolinite intercalation complex can live stably for a long time.
Description
Technical field
The present invention relates to a kind of preparation method of Serine/Kaolinite/organic Intercalation Compounds, especially relate to a kind of lattice parameter d of c-axis layer direction
001=1.0nm hydration kaolinite is that intercalation presoma is with the Serine/Kaolinite/organic Intercalation Compounds of preparation and preparation method.
Background technology
Kaolinite is a kind of important nonmetal mineral resource, primarily of kaolinite race mineral compositions such as small sheet, tubulose, laminated, is industrially widely used in papermaking, pottery, paint, rubber, plastics, field of petrochemical industry.Kaolinite (Al
2si
2o
5(OH)
4) be a kind of typical 1:1 type layered silicate, be made up of as periodic arrangement on c-axis direction, between layers mainly through hydrogen bonded silicon-oxy tetrahedron lamella and alumina octahedral lamella.Under certain condition, some molecule can overcome interlaminar action power and insert kaolinite interlayer, and does not destroy its original laminate structure, and this process is called intercalation.
Kaolinite/organic Intercalation Compounds is the focus of industry research always, at present, research direction both at home and abroad about Kaolinite/organic Intercalation Compounds mainly contains two focuses: the UV absorber being neokaoline intercalated compound is on the one hand the application of Kaolinite/organic Intercalation Compounds in frontier on the other hand.This matrix material is different from traditional matrix material, and its interlayer is nano-area, can produce the special property not available for some parents under the synergy of each component therein.Owing to there is a large amount of hydroxyls in kaolinite structure and not having tradable ion, thus different from the polynite of expanded clay mineral, kaolinic intercalated compound shows special high-performance in forming process.
Further, kaolinite has excellent biocompatibility, chemistry and thermostability, aboundresources, low price, and its special surface and textural property, be with a wide range of applications in medical, studies have reported that and can be used as anti-biotic material, skincare material and hemostatic material etc.By introducing functional molecular at kaolinite interlayer, the intercalated compound obtained not only has the function of kaolinite itself, also has the function of intercalation thing concurrently, thus obtains the mixture of function enhancing.
For example, after drug molecule enters into kaolinite interlayer region, its stability and activity can keep, and at interlayer mostly in monolayer distribution, can improve solvability and the perviousness of drug molecule.This kind of medicine, as protein and peptide medicine, physico-chemical property is unstable, the directly oral destruction being subject to gi tract pH, flora and enzyme system, or the derivative toxic side effect as Serine is large, can not be directly oral, and kaolinite interlayer region is these drug molecules provides desirable environment, avoids above problem.
But, general molecule is difficult to directly enter kaolinite interlayer, only have the organic molecule intercalation as direct in energy such as methane amide, methyl-sulphoxide, hydrazine hydrate, urea that the polarity of only a few is strong, other molecules then need to enter interlayer through displacement again by corresponding intercalation presoma.Usually the intercalated molecule in these presomas has stronger toxicity, as adopted it as presoma during preparation, on the one hand to human body poisonous and harmful; On the other hand, intercalated molecule polarity in these presomas is strong, also namely strong with kaolinite interlaminar action power, thus the replacement(metathesis)reaction cycle is also very long, as passed through methyl-sulphoxide/Kaolinite/organic Intercalation Compounds, N, dinethylformamide/Kaolinite/organic Intercalation Compounds is as precursor power succinimide/Kaolinite/organic Intercalation Compounds, glutarimide/Kaolinite/organic Intercalation Compounds, and preparation needs several days even time of some months.Thus Kaolinite/organic Intercalation Compounds preparation and the application at field of medicaments can be limited.So, preparing nontoxic Kaolinite/organic Intercalation Compounds presoma to replace Kaolinite/organic Intercalation Compounds required for preparation by being one of current important process, in medical applications field, there is important practical significance and social value especially.
From medicine, Serine has a wide range of applications in fields such as medicine, makeup.In medical, be widely used in configuration amino acid fluid infusion, particularly third generation amino acid transfusion and accessory substance; And for the synthesis of multiple Serine derivative, comprise anticancer, acquired immune deficiency syndrome (AIDS) new drug and genetically engineered protected amino acid etc.The derivative seromycin of Serine is a kind of microbiotic, can be used for treating tuberculosis; Azaserine is a kind of carcinostatic agent, is usually used in treating tumour, simultaneously as the metabolic antagonist of glutamine, can be used for treatment acute leukemia and Ke Jie king's evil.Meanwhile, Serine is the important intermediate of synthetic proteins polypeptide drug, and protein and peptide drugs has a wide range of applications in medical diagnosis on disease, treatment or prevention.In makeup, Serine is one of important natural Moisture factor (NMF), and keratoderma keeps the key player of moisture; it also has skin makeup function, and water conservation is antibacterial; buffering, tensio-active agent provide protection, and some is conducive to the physiological action of antibody.Therefore, prepare Serine/Kaolinite/organic Intercalation Compounds makeup and medical in have a wide range of applications and be worth.
But the minimum Van der Waals diameter of Serine is 0.56nm, also namely its molecular dimension is comparatively large, the d in fact will kaolinite c-axis direction lattice parameter being made from former stone after Serine inserts kaolinite layer
001=0.74nm becomes d
001=1.14nm, will allow Serine directly insert original kaolinite as seen, then must by interlamellar spacing significantly by d
001=0.74nm struts d
001=1.14nm, this obviously needs very high energy, and thus Serine directly cannot insert kaolinite equally.But, if consider utilize a kind of Kaolinite/organic Intercalation Compounds for presoma by replace way prepare Serine/Kaolinite/organic Intercalation Compounds, presoma c-axis direction lattice parameter value and Serine is wherein kept to insert lattice parameter thinking relatively in c-axis direction after kaolinite layer, then replace required energy will significantly decline, be expected to realize Serine to insert kaolinite.
Know, hydration kaolinite is the harmless Kaolinite/organic Intercalation Compounds of a kind of totally nontoxic, if using hydration kaolinite as intercalation presoma, the Kaolinite/organic Intercalation Compounds of preparation containing drug molecule, then its intercalated compound will be that one is both nontoxic, there is again the Thermosensitive Material Used for Controlled Releasing of Medicine of required medical function, will have wide practical use and market potential in medical.And in hydration kaolinite, have a kind of c-axis direction lattice parameter d
001the intercalated compound of=1.0nm, the interlamellar spacing d as seen after its intercalation
001interlamellar spacing d after=1.0nm and Serine intercalation
001=1.14nm is very close, is very likely that one can be used for intercalation Serine hydration kaolinite presoma preferably.Further, water molecules is formed hydrogen bond by hydroxyl and kaolinite interlayer hydroxyl and formed stable intercalated compound, and simultaneously containing three kinds of groups such as amino, carboxyl and hydroxyls in Serine molecule, and it becomes the quantity of key group and becomes key reactive force relatively much bigger than the effect of water molecules and kaolinite interlayer, it is more stable that the Serine/Kaolinite/organic Intercalation Compounds formed compares hydration kaolinite, so Serine molecule may be replaced the water in this hydration kaolinite and form Serine/Kaolinite/organic Intercalation Compounds theoretically.
Prepared layer spacing is d
001the hydration kaolinite method of=1.0nm is a lot, Gardolinski, JE etc. with DMSO/ Kaolinite/organic Intercalation Compounds for precursor power d
001=1.0nm hydration kaolinite, Makoto Sato etc. are with d
001=0.85nm hydration kaolinite is precursor power d
001=1.0nm hydration kaolinite etc.The present invention utilizes and prepares d through the transition of ethylene glycol intercalation mesophase spherule
001=1.0nm hydration kaolinite, and obtain Serine/Kaolinite/organic Intercalation Compounds with this success through replacing water molecule.
But although as mentioned above, the replaceable water molecules of Serine molecule and insert kaolinite interlayer, owing to also can be subject to the impact of many-sided kinetic factor in intercalation process, thus can have influence on the size of actual intercalation rate.Particularly in this reaction system, along with the difference of Serine strength of solution, temperature, Serine originally can produce different crystallizations before successfully inserting kaolinite.On the one hand, when Serine strength of solution is relative with temperature of reaction improve time, the amount of the Serine crystal of separating out also increases thereupon, although also i.e. at high temperature intercalation speed, but crystallization speed is faster, Serine molecule between participation interposed layer might not be increased, so intercalation rate is not high by crystallization affects.On the other hand, when concentration and temperature relatively low time, although the Serine crystal of separating out before intercalation is relatively also less, because strength of solution own is low and temperature of reaction is also low, so intercalation rate is not high yet.But, when in solution, serine concentration is high, and when temperature is reduced, although because low temperature can make the speed between Serine interposed layer slower, but because the amount of precipitation of at this moment Serine molecule crystal is relatively also less, also namely retaining the molecular conecentration that can participate in intercalation in the solution can be higher, as long as thus through the reaction of certain hour, just can obtain higher intercalation rate; And when Serine strength of solution is lower, improving temperature of reaction, its Serine crystalline phase separated out is due to relatively also less by the lower impact of strength of solution own, but at this moment intercalation speed improves a lot, and thus intercalation rate also can be improved.
Given this, when the hierarchy of control first reacts for some time at higher concentrations at a lower temperature, obtain by the intercalation effect of contribution of concentration; And consider that the carrying out with intercalation can make Serine molecule concentration in solution decline gradually, thus then at high temperature react again, obtain the intercalation effect contributed by temperature.This method both ensure that and its shorter reaction times had obtained higher intercalation rate again.This intercalated compound and preparation process thereof, technique is simple, and easy to prepare, the reaction times is short, is convenient to realize industrialization, splits hair propylhomoserin/Kaolinite/organic Intercalation Compounds significant in the application of the association areas such as medicine.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of with 1.0nm hydration kaolinite be intercalation precursor power Serine/Kaolinite/organic Intercalation Compounds and preparation method.The present invention prepares Serine/Kaolinite/organic Intercalation Compounds by the water molecules of the interlayer in Serine hydration kaolinite intercalation presoma.
The object of the invention is to be achieved through the following technical solutions: a kind of Serine/Kaolinite/organic Intercalation Compounds that is intercalation precursor power with 1.0nm hydration kaolinite, Serine enters kaolinite interlayer, and kaolinite interlamellar spacing is by inserting the d before Serine
001=1.0nm is extended to the d after inserting Serine
001=1.14nm, intercalation rate is 90% ~ 100%; Serine is monolayer alignment at kaolinite interlayer to be parallel to kaolinite lamella mode, and its carboxyl and kaolinic internal surface hydroxyl form hydrogen bond, aminoly forms hydrogen bond with the Sauerstoffatom of kaolinite silica layer;-OH the group of Serine slips in space, kaolinite silicon-oxy tetrahedron compound three hole; Described Serine/Kaolinite/organic Intercalation Compounds can long-time stable exist in atmosphere.
The preparation method of above-mentioned Serine/Kaolinite/organic Intercalation Compounds, comprises the following steps:
(1) Serine crystal is placed in water through stirring and dissolving, obtain the pure clear Serine aqueous solution, strength of solution is 0.5 ~ 2mol/L;
(2) be d by interlamellar spacing
001the Serine aqueous solution that the hydration kaolinite powder of=1.0nm and step 1 obtain, the mass volume ratio of hydration kaolinite powder and the Serine aqueous solution is 1:100(g/mL), then first react after 2 ~ 3min through magnetic agitation between 10 ~ 20 DEG C, adjust the temperature to 20 ~ 60 DEG C again, continue stirring reaction 1 ~ 2min, obtain resultant of reaction mixing solutions;
(3) by the resultant of reaction mixing solutions of step 2 through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
Further, described interlamellar spacing is d
001the hydration kaolinite powder of=1.0nm can be prepared by following sub-step:
(2.1) be d by 1g interlamellar spacing
001the hydration kaolinite of=0.84nm mixes with 50mL ethylene glycol solution, at room temperature after continuously stirring 6 ~ 24h, obtain reacting the ethylene glycol/Kaolinite/organic Intercalation Compounds mixing solutions generated, by mixing solutions centrifugation, obtain ethylene glycol/Kaolinite/organic Intercalation Compounds powder;
(2.2) by the aqueous solution of 1g ethylene glycol/Kaolinite/organic Intercalation Compounds powder and 50mL, at room temperature after continuously stirring 2h, obtaining interlamellar spacing is d
001=1.0nm hydration kaolinite mixing solutions, by mixing solutions centrifugation, obtains 1.0nm hydration kaolinite powder.
The beneficial effect that the present invention has compared with background technology is:
1, d is adopted
001=1.0nm hydration kaolinite is intercalation presoma, and interlayer only containing water molecules, can not cause environmental pollution, harmless to human non-toxic, is a kind of environmentally friendly presoma.
2, Serine d
001=1.0nm hydration kaolinic middle water molecular reaction speed is fast, and the cycle is short, complete reaction can obtain Serine/Kaolinite/organic Intercalation Compounds in 4min.
3, the technique preparing Serine/Kaolinite/organic Intercalation Compounds is simple, low for equipment requirements, only needs the displacement of simple liquid phase, is convenient to industrialization for actual production.
4, the Serine that the present invention is used has a wide range of applications in fields such as medicine, makeup.Serine/the Kaolinite/organic Intercalation Compounds obtained can be used as makeup, is also that the preparation of the Kaolinite/organic Intercalation Compounds slow release product of serine derivative medicine and protein and peptide drugs lays the foundation.The present invention expands kaolinic range of application, is expected to be applied in fields such as medicine, beauty and skin cares.
Embodiment
The present invention, comprises the following steps for the method for intercalation precursor power Serine/Kaolinite/organic Intercalation Compounds with 1.0nm hydration kaolinite:
1, Serine crystal is placed in water through stirring and dissolving, obtain the pure clear Serine aqueous solution, strength of solution is 0.5 ~ 2mol/L.
2, be d by interlamellar spacing
001the Serine aqueous solution that the hydration kaolinite powder of=1.0nm and step 1 obtain, the mass volume ratio of hydration kaolinite powder and the Serine aqueous solution is 1:100(g/mL), then first react after 2 ~ 3min through magnetic agitation between 10 ~ 20 DEG C, adjust the temperature to 20 ~ 60 DEG C again, continue stirring reaction 1 ~ 2min, obtain resultant of reaction mixing solutions.
Interlamellar spacing is d
001the hydration kaolinite powder of=1.0nm can be prepared by following sub-step:
2.1, be d by 1g interlamellar spacing
001the hydration kaolinite of=0.84nm mixes with 50mL ethylene glycol solution, at room temperature after continuously stirring 6 ~ 24h, obtain reacting the ethylene glycol/Kaolinite/organic Intercalation Compounds mixing solutions generated, by mixing solutions centrifugation, obtain ethylene glycol/Kaolinite/organic Intercalation Compounds powder.Interlamellar spacing is d
001the name that the hydration kaolinite of=0.84nm can be applied on June 14th, 2012 by applicant is called that " hydrazine hydrate-Kaolinite/organic Intercalation Compounds prepares d
001the kaolinic method of=0.84nm hydration ", number of patent application be 201210195865.9 patent of invention prepare.
2.2, by the aqueous solution of 1g ethylene glycol/Kaolinite/organic Intercalation Compounds powder and 50mL, at room temperature after continuously stirring 2h, obtaining interlamellar spacing is d
001=1.0nm hydration kaolinite mixing solutions, by mixing solutions centrifugation, obtains d
001=1.0nm hydration kaolinite powder.
3, by the resultant of reaction mixing solutions of step 2 through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
Serine/the Kaolinite/organic Intercalation Compounds prepared by above-mentioned steps shows through X-ray diffraction, infrared spectra and scanning electron microscope analysis and series of experiments result, and Serine enters kaolinite interlayer and obtains Serine/Kaolinite/organic Intercalation Compounds: kaolinite interlamellar spacing is by d when originally inserting water
001=1.0nm is extended to the d after inserting Serine
001=1.14nm, intercalation rate can reach 90% ~ 100%, and Serine is monolayer alignment at kaolinite interlayer to be parallel to kaolinite lamella mode, and its carboxyl and kaolinic internal surface hydroxyl form hydrogen bond, aminoly forms hydrogen bond with the Sauerstoffatom of kaolinite silica layer.-OH the group of Serine slips in space, kaolinite silicon-oxy tetrahedron compound three hole.Serine/Kaolinite/organic Intercalation Compounds can long-time stable exist in atmosphere.
Describe the present invention in detail according to embodiment below, object of the present invention and effect will become more obvious.
embodiment 1
(1) Serine crystal is placed in water through stirring and dissolving, obtains the pure clear Serine aqueous solution (1), wherein control strength of solution at 1.0mol/L.
(2) by the d of every 1g
001it is in the 1.0mol/L Serine aqueous solution (1) that=1.0nm hydration kaolinite powder joins 100ml concentration, then first react after 2min through magnetic agitation between 10 DEG C, adjust the temperature to 30 DEG C again, continue stirring reaction 2min, obtain resultant of reaction mixing solutions (2).
(3) by resultant of reaction mixing solutions (2) through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
The interlamellar spacing of the Serine/Kaolinite/organic Intercalation Compounds prepared by above-mentioned steps is from the d of former stone
001=0.72nm expands d to
001=1.14nm, the Serine obtained/Kaolinite/organic Intercalation Compounds intercalation rate is 91%.
embodiment 2
(1) Serine crystal is placed in water through stirring and dissolving, obtains the pure clear Serine aqueous solution (1), wherein control strength of solution at 1.5mol/L.
(2) by the d of every 1g
001it is in the 1.5mol/L Serine aqueous solution (1) that=1.0nm hydration kaolinite powder joins 100ml concentration, then first react after 3min through magnetic agitation between 15 DEG C, adjust the temperature to 40 DEG C again, continue stirring reaction 2min, obtain resultant of reaction mixing solutions (2).
(3) by resultant of reaction mixing solutions (2) through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
The interlamellar spacing of the Serine/Kaolinite/organic Intercalation Compounds prepared by above-mentioned steps is from the d of former stone
001=0.72nm expands d to
001=1.14nm, the Serine obtained/Kaolinite/organic Intercalation Compounds intercalation rate is 100%.
embodiment 3
(1) Serine crystal is placed in water through stirring and dissolving, obtains the pure clear Serine aqueous solution (1), wherein control strength of solution at 2.0mol/L.
(2) by the d of every 1g
001it is in the 2.0mol/L Serine aqueous solution (1) that=1.0nm hydration kaolinite powder joins 100ml concentration, then first react after 3min through magnetic agitation between 20 DEG C, adjust the temperature to 60 DEG C again, continue stirring reaction 1min, obtain resultant of reaction mixing solutions (2).
(3) by resultant of reaction mixing solutions (2) through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
The interlamellar spacing of the Serine/Kaolinite/organic Intercalation Compounds prepared by above-mentioned steps is from the d of former stone
001=0.72nm expands d to
001=1.14nm, the Serine obtained/Kaolinite/organic Intercalation Compounds intercalation rate is 100%.
Embodiment 4
(1) Serine obtained by 1g/Kaolinite/organic Intercalation Compounds powder and 100mL aqueous solution, obtain the reaction system of Serine/Kaolinite/organic Intercalation Compounds and the aqueous solution.
(2) by the reaction system of Serine/Kaolinite/organic Intercalation Compounds and the aqueous solution at room temperature through continuously stirring 2h, obtain hydration kaolinite mixing solutions.
(3) by hydration kaolinite mixing solutions through centrifugation, remove supernatant liquid, obtain hydration kaolinite powder.
Can obtain kaolinite by above-mentioned steps, prove that Serine can from Serine/slow deintercalation occurs Kaolinite/organic Intercalation Compounds interlayer until completely dissolve, this is a medicament slow release process.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (2)
1., with a preparation method for the 0nm hydration kaolinite Serine/Kaolinite/organic Intercalation Compounds that is intercalation precursor power, in described Serine/Kaolinite/organic Intercalation Compounds, Serine enters kaolinite interlayer, and kaolinite interlamellar spacing is by inserting the d before Serine
001=1.0nm is extended to the d after inserting Serine
001=1.14nm, intercalation rate is 90% ~ 100%; Serine is monolayer alignment at kaolinite interlayer to be parallel to kaolinite lamella mode, and its carboxyl and kaolinic internal surface hydroxyl form hydrogen bond, aminoly forms hydrogen bond with the Sauerstoffatom of kaolinite silica layer;-OH the group of Serine slips in space, kaolinite silicon-oxy tetrahedron compound three hole; Described Serine/Kaolinite/organic Intercalation Compounds can long-time stable exist in atmosphere; It is characterized in that, the method comprises the following steps:
(1) Serine crystal is placed in water through stirring and dissolving, obtain the pure clear Serine aqueous solution, strength of solution is 0.5 ~ 2mol/L;
(2) be d by interlamellar spacing
001the Serine aqueous solution that the hydration kaolinite powder of=1.0nm and step 1 obtain, the mass volume ratio of hydration kaolinite powder and the Serine aqueous solution is 1:100g/mL, then first react after 2 ~ 3min through magnetic agitation between 10 ~ 20 DEG C, adjust the temperature to 20 ~ 60 DEG C again, continue stirring reaction 1 ~ 2min, obtain resultant of reaction mixing solutions;
(3) by the resultant of reaction mixing solutions of step 2 through centrifugation, remove supernatant liquid, finally obtain Serine/Kaolinite/organic Intercalation Compounds powder.
2. method according to claim 1, is characterized in that, described interlamellar spacing is d
001the hydration kaolinite powder of=1.0nm is prepared by following sub-step:
(2.1) be d by 1g interlamellar spacing
001the hydration kaolinite of=0.84nm mixes with 50mL ethylene glycol solution, at room temperature after continuously stirring 6 ~ 24h, obtain reacting the ethylene glycol/Kaolinite/organic Intercalation Compounds mixing solutions generated, by mixing solutions centrifugation, obtain ethylene glycol/Kaolinite/organic Intercalation Compounds powder;
(2.2) by the aqueous solution of 1g ethylene glycol/Kaolinite/organic Intercalation Compounds powder and 50mL, at room temperature after continuously stirring 2h, obtaining interlamellar spacing is d
001=1.0nm hydration kaolinite mixing solutions, by mixing solutions centrifugation, obtains 1.0nm hydration kaolinite powder.
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