CN106582564A - Attapulgite-polyacrylic acid nanocomposite gel with high adsorptivity and preparation method thereof - Google Patents

Attapulgite-polyacrylic acid nanocomposite gel with high adsorptivity and preparation method thereof Download PDF

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Publication number
CN106582564A
CN106582564A CN201610988766.4A CN201610988766A CN106582564A CN 106582564 A CN106582564 A CN 106582564A CN 201610988766 A CN201610988766 A CN 201610988766A CN 106582564 A CN106582564 A CN 106582564A
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attapulgite
parts
nano
polyacrylic acid
solution
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CN201610988766.4A
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张志军
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ANHUI BOSHUO TECHNOLOGY Co Ltd
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ANHUI BOSHUO TECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/265Synthetic macromolecular compounds modified or post-treated polymers
    • B01J20/267Cross-linked polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047Gels

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses attapulgite-polyacrylic acid nanocomposite gel with the high adsorptivity and a preparation method thereof. The attapulgite-polyacrylic acid nanocomposite gel is characterized by being prepared from, by weight, 2-4 parts of nano-zeolite powder, 5-10 parts of attapulgite, 1-2 parts of silicon dioxide, 15-20 parts of a hydrochloric acid solution, 30-40 parts of a zinc sulfate solution, an appropriate amount of absolute ethyl alcohol, 1-3 parts of nylon fibers, 2-5 parts of a silane coupling agent KH-570, 2-5 parts of a silane coupling agent KH-550, 2-3 parts of chitosan, 0.4-1 part of cerous nitrate, 5-10 parts of acrylic acid, an appropriate amount of nitrogen and an appropriate amount of distilled water. According to the attapulgite-polyacrylic acid nanocomposite gel with the high adsorptivity and the preparation method thereof, chitosan added in a cooperative mode is rich in amino groups, and therefore not only can the amino groups be provided to be grafted on attapulgite to participate in crosslinking to enhance the stability of the network structure of the gel, but also the carrier adsorption amount of carriers can be increased due to the fact that chitosan has the very good adsorptivity; by adding the nano-zeolite powder and the like in a cooperative mode, the advantages of being good in adsorption performance and high in strength are given to the material.

Description

A kind of strong attapulgite of adsorptivity/polyacrylic acid nano pluralgel and its preparation Method
Technical field
The present invention relates to a kind of attapulgite carrier and its preparation, more particularly to a kind of strong attapulgite of adsorptivity/poly- Acrylate/nano pluralgel and preparation method thereof.
Background technology
Pharmaceutical carrier discharges and targeted system can reduce drug degradation and loss, reduces side effect, improves biological utilisation Degree, thus its research is increasingly taken seriously.High molecular surfactant is due to the amphipathic structure of its uniqueness, Ke Yijin Row self assembly, forms various forms of aggregations, such as micelle, microemulsion, gel, liquid crystal, vesicle.These aggregations have bag The ability of drug molecule is carried, while and have good permeability to film, become the important research field of pharmaceutical carrier.Attapulgite It is a kind of with attapulgite as key component, the ore deposit of zeopan containing Shuifu County with specialty fibers shape Crystal structural morphology Thing.Due to its excellent adsorptivity, ion exchange, rheological characteristic, catalytic and plasticity, and it is applied to prepare pharmaceutical carrier.
Zhu Longxiang is in its master thesis《In-situ polymerization prepares the gel in attapulgite/polymer nanocomposites Phenomenon and application》In, Nanometer composite hydrogel is prepared for using attapulgite and acrylic acid, but it makes as pharmaceutical carrier With also there is a problem that carrying attached amount, antibiotic property, slow-releasing is not good enough.
The content of the invention
Think deeply based on more than, the present invention is intended to provide a kind of carry the attached pharmaceutical carrier that amount is big, antibiotic property is good with nano combined Hydrogel, and preparation method thereof.
The technical problem to be solved is realized using following technical scheme:
The strong attapulgite of a kind of adsorptivity/polyacrylic acid nano pluralgel, it is characterised in that be by the original of following weight portion Material is made:
Nano zeolite powder 2-4, attapulgite 5-10, silica 1-2, hydrochloric acid solution 15-20, solution of zinc sulfate 30-40 are anhydrous Appropriate amount of ethanol, nylon fiber 1-3, Silane coupling reagent KH-570 2-5, silane resin acceptor kh-550 2-5, shitosan 2-3, nitric acid Cerium 0.4-1, acrylic acid 5-10, appropriate nitrogen distills appropriate amount of water;
The concentration of hydrochloric acid solution is 2-6mol/L;Solution of zinc sulfate is 0.5-1mol/L.
The strong attapulgite of described a kind of adsorptivity/polyacrylic acid nano pluralgel and preparation method thereof, its feature It is to be made up of following steps:
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, in being scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, add nano zeolite powder, silicon dioxide, immersion 2-3h, obtains rich in silicone hydroxyl, and adsorbs the attapulgite nano stick crystal of zinc ion;
B. step a gained attapulgite nano stick crystal is distributed in dehydrated alcohol, adds Silane coupling reagent KH-570, silane idol Connection agent KH-550, shitosan, nylon fiber, after ultrasonic disperse 1-3h, 60-90 DEG C of backflow 20-26h, with anhydrous after the completion of reaction Washing with alcohol 2-5 time, after being dried, obtains carbon-carbon double bond grafting and amino grafting, shitosan, the attapulgite of nylon fiber absorption is received Rice rod is brilliant;
C. step b gained attapulgite nano stick crystal is distributed in distilled water, after ultrasonic disperse 1-2h, adds cerous nitrate, propylene Acid, under the conditions of nitrogen protection, magnetic agitation, in 50-80 DEG C 18-25h is reacted, and is washed away unreacted acrylic acid with distilled water and is gathered Acrylic acid, obtains final product the attapulgite/polypropylene composite materials gel of shitosan reinforcement.
The strong attapulgite of described a kind of adsorptivity/polyacrylic acid nano pluralgel and preparation method thereof, its feature Be, the drying condition in step b be 30-50 DEG C at be vacuum dried 20-26h.
The invention has the beneficial effects as follows:Attapulgite is processed with hydrochloric acid solution and solution of zinc sulfate so that attapulgite table Face is rich in silicone hydroxyl, is that the graft modification of next step is prepared, while the zinc ion of absorption has the effect of sterilization, enables carrier Preferably apply in terms of medical treatment;With silane resin acceptor kh-550 and KH-570 it is attapulgite modified after, obtain amino and carbon carbon The attapulgite of double bond grafting;Under the catalytic action of cerous nitrate, acrylic acid is gone back on attapulgite nano stick crystal surface by oxidation Original reaction causes polymerization, and polyreaction is then crosslinked with the attapulgite of grafted amino group and carbon-carbon double bond, forms three dimensional network The Nanometer composite hydrogel of network structure;Meanwhile, the shitosan of addition is rich in amino, not only can provide amino and be grafted to attapulgite On soil, crosslinking is participated in, strengthen the stability of its network structure, while shitosan has good adsorptivity, carrier can be increased The attached amount of load;Coordinate nano zeolite powder etc. of addition, the characteristics of give good material absorption property and high intensity.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.
Embodiment
The strong attapulgite of a kind of adsorptivity/polyacrylic acid nano pluralgel, it is characterised in that be by following weight portion Raw material make:
Nano zeolite powder 4, attapulgite 10, silicon dioxide 2, hydrochloric acid solution 20, solution of zinc sulfate 40, appropriate dehydrated alcohol, Buddhist nun Imperial fiber 3, Silane coupling reagent KH-570 5, silane resin acceptor kh-550 5, shitosan 3, cerous nitrate 1, acrylic acid 10, nitrogen is fitted Amount, distills appropriate amount of water;
The concentration of hydrochloric acid solution is 2-6mol/L;Solution of zinc sulfate is 0.5-1mol/L.
The strong attapulgite of described a kind of adsorptivity/polyacrylic acid nano pluralgel and preparation method thereof, its feature It is to be made up of following steps:
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, in being scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, add nano zeolite powder, silicon dioxide, immersion 2-3h, obtains rich in silicone hydroxyl, and adsorbs the attapulgite nano stick crystal of zinc ion;
B. step a gained attapulgite nano stick crystal is distributed in dehydrated alcohol, adds Silane coupling reagent KH-570, silane idol Connection agent KH-550, shitosan, nylon fiber, after ultrasonic disperse 1-3h, 60-90 DEG C of backflow 20-26h, with anhydrous after the completion of reaction Washing with alcohol 2-5 time, after being dried, obtains carbon-carbon double bond grafting and amino grafting, shitosan, the attapulgite of nylon fiber absorption is received Rice rod is brilliant;
C. step b gained attapulgite nano stick crystal is distributed in distilled water, after ultrasonic disperse 1-2h, adds cerous nitrate, propylene Acid, under the conditions of nitrogen protection, magnetic agitation, in 50-80 DEG C 18-25h is reacted, and is washed away unreacted acrylic acid with distilled water and is gathered Acrylic acid, obtains final product the attapulgite/polypropylene composite materials gel of shitosan reinforcement.
The strong attapulgite of described a kind of adsorptivity/polyacrylic acid nano pluralgel and preparation method thereof, its feature Be, the drying condition in step b be 30-50 DEG C at be vacuum dried 20-26h.
The present invention technical parameter be:When pH value is 7.0, to the adsorbance of the methylene blue solution of 90.0mg/L >= 302.0 mg/g。

Claims (3)

1. the strong attapulgite of a kind of adsorptivity/polyacrylic acid nano pluralgel, it is characterised in that be by following weight portion Raw material is made:
Nano zeolite powder 2-4, attapulgite 5-10, silica 1-2, hydrochloric acid solution 15-20, solution of zinc sulfate 30-40 are anhydrous Appropriate amount of ethanol, nylon fiber 1-3, Silane coupling reagent KH-570 2-5, silane resin acceptor kh-550 2-5, shitosan 2-3, nitric acid Cerium 0.4-1, acrylic acid 5-10, appropriate nitrogen distills appropriate amount of water;
The concentration of hydrochloric acid solution is 2-6mol/L;Solution of zinc sulfate is 0.5-1mol/L.
2. a kind of strong attapulgite of adsorptivity according to claim 1/polyacrylic acid nano pluralgel and its preparation Method, it is characterised in that be made up of following steps:
A. attapulgite is toasted into 1-3h at 120-160 DEG C, after removing organic compound therein, in being scattered in distilled water, Add hydrochloric acid solution, solution of zinc sulfate to be activated and ion exchange absorption, add nano zeolite powder, silicon dioxide, immersion 2-3h, obtains rich in silicone hydroxyl, and adsorbs the attapulgite nano stick crystal of zinc ion;
B. step a gained attapulgite nano stick crystal is distributed in dehydrated alcohol, adds Silane coupling reagent KH-570, silane idol Connection agent KH-550, shitosan, nylon fiber, after ultrasonic disperse 1-3h, 60-90 DEG C of backflow 20-26h, with anhydrous after the completion of reaction Washing with alcohol 2-5 time, after being dried, obtains carbon-carbon double bond grafting and amino grafting, shitosan, the attapulgite of nylon fiber absorption is received Rice rod is brilliant;
C. step b gained attapulgite nano stick crystal is distributed in distilled water, after ultrasonic disperse 1-2h, adds cerous nitrate, propylene Acid, under the conditions of nitrogen protection, magnetic agitation, in 50-80 DEG C 18-25h is reacted, and is washed away unreacted acrylic acid with distilled water and is gathered Acrylic acid, obtains final product the attapulgite/polypropylene composite materials gel of shitosan reinforcement.
3. a kind of strong attapulgite of adsorptivity according to claim 2/polyacrylic acid nano pluralgel and its preparation Method, it is characterised in that the drying condition in step b be 30-50 DEG C at be vacuum dried 20-26h.
CN201610988766.4A 2016-11-10 2016-11-10 Attapulgite-polyacrylic acid nanocomposite gel with high adsorptivity and preparation method thereof Withdrawn CN106582564A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107935573A (en) * 2017-11-28 2018-04-20 芜湖上水源环保科技有限公司 A kind of microbiological free air purifying filter element preparation method of low cost
CN108905991A (en) * 2018-07-02 2018-11-30 仲恺农业工程学院 A kind of chitosan-polyacrylic acid/attapulgite composite material preparation method
CN111013547A (en) * 2019-12-25 2020-04-17 艾波达(南通)环保科技有限公司 Composite heavy metal adsorbent and preparation method thereof
CN113351183A (en) * 2021-06-16 2021-09-07 西安理工大学 Magnetic response type nylon adsorption material and preparation method thereof

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CN102500158A (en) * 2011-11-29 2012-06-20 无锡格瑞普尔膜科技有限公司 Preparation method for high-efficiency filter medium with adion exchanging function and membrane filtering function
CN103496711A (en) * 2013-09-10 2014-01-08 叶香雄 Preparation method of antibacterial attapulgite
CN103614804A (en) * 2013-11-22 2014-03-05 东华大学 Preparation method of nylon 66/attapulgite clay nano-composite fiber
CN103724633A (en) * 2012-10-15 2014-04-16 中国科学院兰州化学物理研究所 Granular hydrogel

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102500158A (en) * 2011-11-29 2012-06-20 无锡格瑞普尔膜科技有限公司 Preparation method for high-efficiency filter medium with adion exchanging function and membrane filtering function
CN103724633A (en) * 2012-10-15 2014-04-16 中国科学院兰州化学物理研究所 Granular hydrogel
CN103496711A (en) * 2013-09-10 2014-01-08 叶香雄 Preparation method of antibacterial attapulgite
CN103614804A (en) * 2013-11-22 2014-03-05 东华大学 Preparation method of nylon 66/attapulgite clay nano-composite fiber

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107935573A (en) * 2017-11-28 2018-04-20 芜湖上水源环保科技有限公司 A kind of microbiological free air purifying filter element preparation method of low cost
CN108905991A (en) * 2018-07-02 2018-11-30 仲恺农业工程学院 A kind of chitosan-polyacrylic acid/attapulgite composite material preparation method
CN111013547A (en) * 2019-12-25 2020-04-17 艾波达(南通)环保科技有限公司 Composite heavy metal adsorbent and preparation method thereof
CN113351183A (en) * 2021-06-16 2021-09-07 西安理工大学 Magnetic response type nylon adsorption material and preparation method thereof

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