CN102499249A - Sustained-release penicillin anion intercalation hydrotalcite material as well as preparation and application thereof - Google Patents
Sustained-release penicillin anion intercalation hydrotalcite material as well as preparation and application thereof Download PDFInfo
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- CN102499249A CN102499249A CN2011102905353A CN201110290535A CN102499249A CN 102499249 A CN102499249 A CN 102499249A CN 2011102905353 A CN2011102905353 A CN 2011102905353A CN 201110290535 A CN201110290535 A CN 201110290535A CN 102499249 A CN102499249 A CN 102499249A
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Abstract
The invention relates to the antibacterial technology, in particular to a sustained-release penicillin anion intercalation hydrotalcite material as well as preparation and application thereof. The hydrotalcite material has the following chemical composition general formula of [M<2+>1-xM<3+>x(OH)2]<x+>(C16H17N2O4S<->)x.nH2O, wherein M<2+> is the divalent metal ion of Mg<2+>, Zn<2+>, Ni<2+>, Fe<2+> or Mn<2+>, M<3+> is the trivalent metal ion of Al<3+>, Cr<3+>, Fe<3+>, V<3+>, Co<3+>, Ga<3+> or Ti<3+>, the molar ratio of M<2+>/M<3+> is 1.6-4.5, and x is more than or equal to 0.2 and is less than or equal to 0.4. The invention provides the sustained-release penicillin anion intercalation hydrotalcite material and a preparation method thereof. The material is characterized in that penicillin anions are introduced be among hydrotalcite layers; penicillin anion antibacterial agent is released by exchanging anions in the environment and the penicillin anions among the layers to achieve the antibacterial purpose and obviously improve the light and heat stability of penicillin molecules, and the sustained-release penicillin anion intercalation hydrotalcite material has the possibility of serving as the filler of the antibacterial coating to achieve the function of inhibiting microorganism staining.
Description
Technical field
The present invention relates to antimicrobial technology, a kind of specifically spacetabs type penicillin anion intercalation hydrotalcite material and preparation and application.
Background technology
The appearance of material surface microorganism blanket, it is stained to be referred to as microorganism.This cover layer is referred to as biomembrane.The microbiologic(al) corrosion effect that in marine environment, only produces because of sulfate reducing bacteria makes the production, transportation of petroleum industry and loss that bunkerage suffers every year just reach multi-billion dollar.And according to incompletely statistics, the microbiologic(al) corrosion loss accounts for about 20% of total corrosion loss.
Protective coating is the most frequently used stained means of defence of microorganism, and its function mainly realizes through bactericide.But traditional bactericide is forbidden gradually or is limited the use of owing to high toxicity.Therefore, the new environmentally friendly guard technology of exploitation is imperative.In recent years, the friendly type bactericide of novel environmental is owing to its efficient, green characteristic causes people's extensive concern.But its exist photo and thermal stability poor, process the characteristics that are prone to inactivation after the coating, this has limited its further application.
(layered double hydroxides LDHs) is a kind of typical stratiform anionic clay to hydrotalcite, because it has good interlayer ion interchangeability, has the characteristic of molecule container, has caused people's extensive concern in recent years.
Summary of the invention
The purpose of this invention is to provide a kind of spacetabs type penicillin anion intercalation hydrotalcite material and preparation and application.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of spacetabs type penicillin anion intercalation hydrotalcite material: said hydrotalcite material chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Be Mg
2+, Zn
2+, Ni
2+, Fe
2+Or Mn
2+Bivalent metal ion; M
3+Be Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+Or Ti
3+Trivalent metal ion; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
Said M
2+Be Mg
2+Bivalent metal ion.
Said M
3+Be Al
3+Trivalent metal ion.
Spacetabs type penicillin anion intercalation hydrotalcite preparation methods:
1) with M
2+Soluble-salt and M
3+Soluble-salt, press M
2+/ M
3+Mol ratio is that 2～4 ratio is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M in the mixing salt solution
2+Concentration be 0.10～1.00mol/L, for use;
2) NaOH is dissolved in takes off CO
2Deionized water in be mixed with the aqueous slkali that concentration is 2～6mol/L, for use;
3) with step 1) and step 2) above-mentioned two kinds of solution are at N
2Protection mixes down, and stirred 30～60 minutes;
4) slurries that above-mentioned mixing obtained crystallization 10～16 hours under 120～150 ℃ of conditions is with taking off CO
2Deionized water washing, filter, get the CO that takes off that filter cake joins potassium salt of penicillin
2Deionized water solution at N
2Protection is down in room-temperature ion exchange 24～48 hours, then with taking off CO
2Deionized water washing, filter, with filter cake vacuum drying at room temperature 12～24 hours, obtaining the chemical composition general formula was [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2The penicillin anion intercalation hydrotalcite of O.
Said M
2+Be Mg
2+, Zn
2+, Ni
2+, Fe
2+Or Mn
2+Bivalent metal ion; M
3+Be Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+Or Ti
3+Trivalent metal ion; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
Said solubility divalent metal salt is a nitrate, and the solubility trivalent metal salt is a nitrate.
Said M
2+Be Mg
2+
Said M
3+Be Al
3+
The application of spacetabs type penicillin anion intercalation hydrotalcite material: said hydrotalcite material can be used as antibiotic preparation.Specifically can be the antibiotic preparation of micrococcus lysodeikticus.
Effect of the present invention and advantage are: the invention provides a kind of spacetabs type penicillin anion intercalation hydrotalcite anti-biotic material and preparation method thereof; This material is introduced hydrotalcite layers with the penicillin anion; Reach release penicillin anion antibacterial agent through anion in the environment and the anionic exchange of interlayer penicillin; Reach antibiotic purpose, and significantly improve penicillin molecule photo and thermal stability, be expected to reach the stained function of inhibition microorganism as the filler use of antimicrobial coating.
Description of drawings
The XRD spectra of the anion intercalated Mg-Al LDHs of gained penicillin (Mg/Al=2) that Fig. 1 provides for the embodiment of the invention (abscissa-angle 2 θ wherein, unit is ° (degree); Ordinate-intensity, unit is a.u. (absolute unit)).
(abscissa-wave number, unit is nm to Fig. 2 for the FT-IR spectrogram of the anion intercalated Mg-Al LDHs of gained penicillin (Mg/Al=2) that the embodiment of the invention provided
-1(every nanometer); Ordinate-intensity, unit is a.u. (absolute unit)).
Fig. 3 contains bacteriostasis rate and relation curve release time (abscissa-release time wherein, the min of unit (minute) of different release times in the anion intercalated Mg-AlLDHs of 0.4g/L penicillin (Mg/Al=2) the 3.5%NaCl solution for the embodiment of the invention provided; Ordinate-bacteriostasis rate, the % of unit (percentage)).
Embodiment
Embodiment 1
Said anti-biotic material chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Represent bivalent metal ion Mg
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 2; X is 0.33.
The preparation process:
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Mg (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing salt solution (Mg of 0.75mol/L
2+/ Al
3+=2).NaOH is made into the aqueous slkali of 6mol/L.Salting liquid and aqueous slkali are joined in the four-hole boiling flask behind the vigorous stirring 30min simultaneously, filter, change the gained slurries in the agitated reactor 140 ℃ of hydrothermal crystallizing 10h after the washing.Whole process is led to nitrogen protection.Product cooling, washing, centrifugation are got 7.5g prepared fresh filter cake and are joined the 100mL that contains the 1.86g potassium salt of penicillin and take off CO
2Deionized water solution in room temperature nitrogen protection vigorous stirring ion exchange 24 hours.Then with taking off CO
2Deionized water washing, filter, with filter cake vacuum drying at room temperature 24 hours, obtain the anion intercalated Mg-Al LDHs of penicillin.XRD test shows product has good crystal formation, belongs to hexagonal crystal system, the obvious (see figure 1) of layer structure characteristic of LDH.FT-IR test shows penicillin anion is the main object anion (Fig. 2) of interlayer.
Getting the anion intercalated Mg-Al LDHs of 80mg penicillin (Mg/Al=2) is distributed in the 200mL3.5%NaCl aqueous solution; Magnetic agitation; By certain hour at interval (5,10,20,60 and 180min) get the 4mL supernatant; And the 3.5%NaCl solution of additional equivalent, institute's clear liquid of getting is numbered A, B, C, D and E respectively at the centrifugal 2min of supercentrifuge 10000rpm.Contain the medium (10g/L peptone, 3g/L beef extract, 5g/L NaCl transfer pH to 6.5) get 2mL and to contain micrococcus lysodeikticus (Micrococcus lysodeikticus) respectively in 12 sterilization test tubes.6 of developmental tubes, the application of sample amount is seen table 1; 6 of control tube, the application of sample amount is seen table 2.After putting 30 ℃ of incubators cultivation certain hours then, be blank with the control tube, light path 1cm, mensuration is respectively managed absorbance at the 450nm place, gets three groups of mean values that repeat, the calculating bacteriostasis rate (inhibition rate, IR).
IR％＝(1-OD
sample/OD
control)×100％…………………………(1)
OD in the formula
SampleBe that 1～No. 5 developmental tube is cultivated the absorbance of measuring after 24 hours; OD
ControlBe that No. 0 developmental tube is cultivated the absorbance of measuring after 24 hours.
Table 1 developmental tube application of sample table
Table 2 control tube application of sample table
In 3.5%NaCl solution, add the anti-bacteria test result of the anion intercalated Mg-Al LDHs of penicillin (Mg/Al=2) when discharging different time and show that hydrotalcite can immobilized penicillin anion and prolong and control its release rate, (wherein instrument uses the Japanese D/MAX of company of science 2500 type X-ray diffractometer (XRD) (Cu K to reach the effect (Fig. 3) that suppresses growth of microorganism
αRadiation, λ=1.5406
) the sign product structure.Adopt the U.S.'s Nicolet iS10 of power & light company FFIR (FT-IR) to characterize interlayer object anion species.The U-2900 of HIT ultraviolet-visual spectrometer characterizes absorbance).
Embodiment 2
Said anticorrosive chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Represent bivalent metal ion Mg
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 3; X is 0.25.
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Mg (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing salt solution (Mg of 0.40mol/L
2+/ Al
3+=3).NaOH is made into the aqueous slkali of 4mol/L.Salting liquid and aqueous slkali are joined in the four-hole boiling flask vigorous stirring simultaneously filter after 40 minutes, change in the agitated reactor gained slurries over to 140 ℃ of hydrothermal crystallizings 12 hours after the washing.Whole process is led to nitrogen protection.Product cooling, with water washing, centrifugation, get 8.0g prepared fresh nitrate anion intercalation LDHs precursor and joined in the 100mL water that contains the 1.86g potassium salt of penicillin ion exchange of room temperature nitrogen protection vigorous stirring 36 hours.Washing, centrifugation obtain the anion intercalated Mg-Al LDHs of penicillin (Mg/Al=3).Anti-bacteria test result shows that hydrotalcite can immobilized penicillin anion and prolong and control its release rate, to reach the effect (Fig. 3) that suppresses growth of microorganism.
Embodiment 3
Said anticorrosive chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Represent bivalent metal ion Ni
2+, M
3+Represent trivalent metal ion Al
3+M
2+/ M
3+Mol ratio be 4; X is 0.20.
Experimental water eliminates CO for the secondary deionized water of just having boiled
2, be reflected at N
2Carry out under the atmosphere.Ni (NO
3)
26H
2O and Al (NO
3)
39H
2O is made into the mixing salt solution (Mg of 1.00mol/L
2+/ Al
3+=4).NaOH is made into the aqueous slkali of 2mol/L.Salting liquid and aqueous slkali are joined in the four-hole boiling flask vigorous stirring simultaneously filter after 60 minutes, change in the agitated reactor gained slurries over to 140 ℃ of hydrothermal crystallizings 16 hours after the washing.Whole process is led to nitrogen protection.Product cooling, washing, centrifugation are got 8.5g prepared fresh nitrate anion intercalation LDHs precursor and were joined in the 100mL water that contains the 1.86g potassium salt of penicillin ion exchange of room temperature nitrogen protection vigorous stirring 48 hours.Washing, centrifugation obtain the anion intercalated Ni-Al LDHs of penicillin (Ni/Al=4).Anti-bacteria test result shows that hydrotalcite can immobilized penicillin anion and prolong and control its release rate, to reach the effect (Fig. 3) that suppresses growth of microorganism.
Embodiment 4
Said anticorrosive chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Represent bivalent metal ion Mg
2+, Zn
2+, Ni
2+, Fe
2+, Mn
2+In any, M
3+Represent trivalent metal ion Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+, Ti
3+In any, M
2+/ M
3+Mol ratio be 1.6～4.5 (1.6,2.0,2.5,3,3.6,4,4.2 or 4.5);≤x≤0.4 0.2 (0.2,0.25,0.3,0.35 or 0.4).
The preparation process:
With M
2+Soluble-salt and M
3+Soluble-salt, press M
2+/ M
3+Mol ratio is that the ratio of 2～4 (2,2.5,3,3.5 or 4) is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M
2+Concentration be 0.10～1.00 (0.1,0.3,0.5,0.8 or 1.0) mol/L; NaOH is dissolved in takes off CO
2Deionized water in be mixed with the aqueous slkali that concentration is 2～6 (2.0,2.5,3.0,3.5,4.0,4.5,5.0,5.5 or 6.0) mol/L; With above-mentioned two kinds of solution at N
2Protection is added dropwise to simultaneously down and stirs 30～60 (30,40,50 or 60) minute in the four-hole boiling flask.With the slurries that obtain crystallization 10～16 (10,12,14 or 16) hour under 120～150 (120,130,140 or 150) ℃ condition, with taking off CO
2Deionized water washing, filter.The filter cake of getting 0.70～0.90 (0.70,0.75,0.80,0.85 or 0.90) prepared fresh joins the 100mL that contains the 1.86g potassium salt of penicillin and takes off CO
2Deionized water intermediate ion exchange 24～48 (24,36 or 48) hour, with taking off CO
2Deionized water washing, filter, with filter cake vacuum drying at room temperature 12～24 (12,14,16,18,20,22 or 24) h, obtain penicillin anion intercalation hydrotalcite precursor.
Described solubility divalent metal salt is a nitrate, and the solubility trivalent metal salt is a nitrate.
Claims (9)
1. spacetabs type penicillin anion intercalation hydrotalcite material, it is characterized in that: said hydrotalcite material chemical composition general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2O, M
2+Be Mg
2+, Zn
2+, Ni
2+, Fe
2+Or Mn
2+Bivalent metal ion; M
3+Be Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+Or Ti
3+Trivalent metal ion; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
2. by the described spacetabs type penicillin of claim 1 anion intercalation hydrotalcite material, it is characterized in that: said M
2+Be Mg
2+Bivalent metal ion.
3. by the described spacetabs type penicillin of claim 1 anion intercalation hydrotalcite anti-biotic material, it is characterized in that: said M
3+Be Al
3+Trivalent metal ion.
4. the described spacetabs type penicillin of claim 1 anion intercalation hydrotalcite preparation methods is characterized in that:
1) with M
2+Soluble-salt and M
3+Soluble-salt, press M
2+/ M
3+Mol ratio is that 2～4 ratio is dissolved in and takes off CO
2Deionized water in be made into mixing salt solution, make M in the mixing salt solution
2+Concentration be 0.10～1.00mol/L, for use;
2) NaOH is dissolved in takes off CO
2Deionized water in be mixed with the aqueous slkali that concentration is 2～6mol/L, for use;
3) with step 1) and step 2) above-mentioned two kinds of solution are at N
2Protection mixes down, and stirred 30～60 minutes;
4) slurries that above-mentioned mixing obtained crystallization 10～16 hours under 120～150 ℃ of conditions is with taking off CO
2Deionized water washing, filter, get the CO that takes off that filter cake joins potassium salt of penicillin
2Deionized water solution at N
2Protection is down in room-temperature ion exchange 24～48 hours, then with taking off CO
2Deionized water washing, filter, with filter cake vacuum drying at room temperature 12～24 hours, obtaining the chemical composition general formula was [M
2+ 1-xM
3+ x(OH)
2]
X+(C
16H
17N
2O
4S
-)
xNH
2The penicillin anion intercalation hydrotalcite of O.
5. by the preparation method of the described spacetabs type penicillin of claim 4 anion intercalation hydrotalcite anti-biotic material, it is characterized in that: said M
2+Be Mg
2+, Zn
2+, Ni
2+, Fe
2+Or Mn
2+Bivalent metal ion; M
3+Be Al
3+, Cr
3+, Fe
3+, V
3+, Co
3+, Ga
3+Or Ti
3+Trivalent metal ion; M
2+/ M
3+Mol ratio be 1.6～4.5; 0.2≤x≤0.4.
6. by the preparation method of the described spacetabs type penicillin of claim 5 anion intercalation hydrotalcite anti-biotic material, it is characterized in that: said solubility divalent metal salt is a nitrate, and the solubility trivalent metal salt is a nitrate.
7. by the preparation method of the described spacetabs type penicillin of claim 5 anion intercalation hydrotalcite anti-biotic material, it is characterized in that: said M
2+Be Mg
2+
8. by the preparation method of the described spacetabs type penicillin of claim 5 anion intercalation hydrotalcite anti-biotic material, it is characterized in that: said M
3+Be Al
3+
9. the application of the described spacetabs type penicillin of claim 1 an anion intercalation hydrotalcite material, it is characterized in that: said hydrotalcite material can be used as antibiotic preparation.
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| CN103333681A (en) * | 2013-07-22 | 2013-10-02 | 北京化工大学 | Intercalation material having fluorescent response to frictional force and volatile organic compound and preparation method of intercalation material |
| CN103651564A (en) * | 2012-09-04 | 2014-03-26 | 中国科学院海洋研究所 | Graphene oxide/hydrotalcite composite antibacterial film material and preparation and application of graphene oxide/hydrotalcite composite antibacterial film material |
| CN109016004A (en) * | 2018-08-31 | 2018-12-18 | 广德竹之韵工艺品厂 | A kind of mould proof uvioresistant processing method of bamboo wood |
| CN109266191A (en) * | 2018-08-31 | 2019-01-25 | 广德竹之韵工艺品厂 | A kind of open air bamboo product coating |
| CN109485968A (en) * | 2018-10-29 | 2019-03-19 | 安徽精乐塑业有限公司 | A kind of environment-friendly type food package film |
| CN112724502A (en) * | 2020-12-31 | 2021-04-30 | 常州威材新材料科技有限公司 | Anti-blushing auxiliary agent and application method thereof |
| CN112812368A (en) * | 2020-12-30 | 2021-05-18 | 常州威材新材料科技有限公司 | Antibacterial flame-retardant material and application method thereof |
| CN113598179A (en) * | 2021-09-07 | 2021-11-05 | 淄博职业学院 | Slow-release bactericide suitable for pet breeding environment and preparation method thereof |
| CN113632787A (en) * | 2021-09-07 | 2021-11-12 | 淄博职业学院 | Slow-release bactericide suitable for hospital environment and preparation method thereof |
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| CN103651564A (en) * | 2012-09-04 | 2014-03-26 | 中国科学院海洋研究所 | Graphene oxide/hydrotalcite composite antibacterial film material and preparation and application of graphene oxide/hydrotalcite composite antibacterial film material |
| CN103651564B (en) * | 2012-09-04 | 2015-11-18 | 中国科学院海洋研究所 | A kind of graphene oxide/hydrotalcite composite antibacterial thin films material and Synthesis and applications thereof |
| CN103333681A (en) * | 2013-07-22 | 2013-10-02 | 北京化工大学 | Intercalation material having fluorescent response to frictional force and volatile organic compound and preparation method of intercalation material |
| CN103333681B (en) * | 2013-07-22 | 2014-07-30 | 北京化工大学 | Intercalation material having fluorescent response to frictional force and volatile organic compound and preparation method of intercalation material |
| CN109016004A (en) * | 2018-08-31 | 2018-12-18 | 广德竹之韵工艺品厂 | A kind of mould proof uvioresistant processing method of bamboo wood |
| CN109266191A (en) * | 2018-08-31 | 2019-01-25 | 广德竹之韵工艺品厂 | A kind of open air bamboo product coating |
| CN109485968A (en) * | 2018-10-29 | 2019-03-19 | 安徽精乐塑业有限公司 | A kind of environment-friendly type food package film |
| CN112812368A (en) * | 2020-12-30 | 2021-05-18 | 常州威材新材料科技有限公司 | Antibacterial flame-retardant material and application method thereof |
| CN112812368B (en) * | 2020-12-30 | 2021-08-06 | 常州威材新材料科技有限公司 | Antibacterial flame-retardant material and application method thereof |
| CN112724502A (en) * | 2020-12-31 | 2021-04-30 | 常州威材新材料科技有限公司 | Anti-blushing auxiliary agent and application method thereof |
| CN112724502B (en) * | 2020-12-31 | 2021-09-07 | 常州威材新材料科技有限公司 | Anti-blushing auxiliary agent and application method thereof |
| CN113598179A (en) * | 2021-09-07 | 2021-11-05 | 淄博职业学院 | Slow-release bactericide suitable for pet breeding environment and preparation method thereof |
| CN113632787A (en) * | 2021-09-07 | 2021-11-12 | 淄博职业学院 | Slow-release bactericide suitable for hospital environment and preparation method thereof |
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Application publication date: 20120620 |