CN108014754A - A kind of preparation method of sulfhydryl modified active bentonite molecular sieve - Google Patents
A kind of preparation method of sulfhydryl modified active bentonite molecular sieve Download PDFInfo
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- CN108014754A CN108014754A CN201711061431.9A CN201711061431A CN108014754A CN 108014754 A CN108014754 A CN 108014754A CN 201711061431 A CN201711061431 A CN 201711061431A CN 108014754 A CN108014754 A CN 108014754A
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- bentonite
- molecular sieve
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid 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 surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Silicon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of sulfhydryl modified active bentonite molecular sieve, after sulfuric acid Bentonite with Microwave Heating, chitosan, activated bentonite are carried out using thioacetic acid afterwards sulfhydryl modified, afterwards with gelatin, liquid paraffin mixing ultrasonic disperse, be molded to obtain microballoon, with sodium metasilicate, lye, guiding agent for zeolite heating crystallization, up to sulfhydryl modified active bentonite molecular sieve.Molecular sieve prepared by the present invention is of low cost using bentonite as raw material, and technique is simple, and specific surface area is big, and stability is good, has stronger adsorption capacity.
Description
Technical field
The invention belongs to bentonite processing technique field, and in particular to a kind of system of sulfhydryl modified active bentonite molecular sieve
Preparation Method.
Background technology
Natural montmorillonite in China's applicating history of existing thousands of years, its conventional use be ceramics, refractory material, glass,
Iron ore pellets and drilling mud etc..But expand with the development of science and technology with the continuous of bentonite application field, increasingly need
The processing of high added value is carried out to natural montmorillonite, to improve bentonitic technical indicator, increases bentonitic use value,
To meet the requirement of industrial and agricultural production and scientific research.Generally will first will be swollen currently with the experiment of bentonite synthesis of molecular sieve
Profit soil carries out activation process, it is therefore an objective to destroys bentonitic layer structure, obtains being used for the activated silica of synthesis of molecular sieve
Source and silicon source.
The content of the invention
The present invention provides a kind of preparation method of sulfhydryl modified active bentonite molecular sieve, molecular sieve prepared by the present invention with
Bentonite is raw material, of low cost, and technique is simple, and specific surface area is big, and stability is good, has stronger adsorption capacity.
The present invention is achieved by the following technical solutions：
A kind of preparation method of sulfhydryl modified active bentonite molecular sieve, it is characterised in that comprise the following steps：
（1）Activated bentonite
20-25 parts by weight of bentonite is put into 3-5 times of distilled water, is filtered after uniform stirring after static 4-5 decimals, by filtering
Bentonite ore pulp, which is put into drying box, dries, and adds the sulfuric acid of 40-50 parts by weight 30-60% afterwards, is placed in micro-wave oven in 80-
Filtered after being heated 1-5 minutes under the conditions of 100 DEG C, wash and dried after at 100-110 DEG C, ground the bentonite of drying with mortar
It is stand-by into powdered；
（2）It is sulfhydryl modified
By 5-10 parts by weight chitosan and step（1）After gained bentonite powder adds suitable water stirring and dissolving, 2-5 weights are added dropwise
Part thioacetic acid is measured, is uniformly mixed, addition 1-4 parts by weight water-soluble carbodiimide is small after stirring reaction 2-4 under room temperature, takes out
Mixed solution, dialyses 3 times for 5-15 DEG C in lucifuge, is sealed after freeze-drying, stand-by；
（3）Prepare microballoon
By 2-5 parts by weight gelatin, the paraffin of 20-40 part by weight of liquid shapes, step is instilled with the speed of 3-6mL/min（2）Gained
In thing, disperse after stirring in ultrasonic cleaner, after shaping, then filtered, washed, dried 200 mesh sieve, obtains microballoon, treat
With；
（4）Crystallization
By step（3）Obtained microballoon is oriented to 25-40 parts by weight sodium metasilicate, 20-25 parts by weight lye, 5-13 parts by weight zeolite
Put into after agent in crystallization kettle, be heated to 90-120 DEG C in 30-40 minutes by room temperature, then to be stirred at reflux 8-24 small for heated at constant temperature
When, cooled to room temperature filtering, filtrate is washed with deionized water, and filters, after dry filtrate, up to sulfhydryl modified active bentonite
Molecular sieve.
The step（1）Wash wash 3-4 times to neutrality with methanol, acetone, clear water successively.
The dialysis is that 5mmol/L hydrochloric acid is dialysed with 1%NaCl mixed solutions with after the dialysis once of 5mmol/L hydrochloric acid solutions
Once, then with 1mmol/L hydrochloric acid solutions dialysis twice
The pH value of the adjusting mixed solution is to use 0.5-1mol/L sodium hydroxide solutions.
The drying is one kind in low temperature drying, spray drying, vacuum drying and freeze-drying.
It is an advantage of the invention that：
After the present invention is by sulfuric acid Bentonite with Microwave Heating, mercapto is carried out to chitosan, activated bentonite using thioacetic acid afterwards
Base be modified, afterwards with gelatin, liquid paraffin mixing ultrasonic disperse, be molded to obtain microballoon, with sodium metasilicate, lye, zeolite guiding
Agent heating crystallization, up to sulfhydryl modified active bentonite molecular sieve.Stability of the bentonite in acid solution is low, can destroy its knot
Structure, improves the reactivity of raw material, and under the action of microwave high-frequency electromagnetic field, bentonite polar molecule can be fast with external electromagnetic field
Speed changes polar orientation, and microwave treatment can shorten soak time, it is sulfhydryl modified by mercapto groups be grafted to bentonite surface and
Interlayer, bentonitic absorption property, the carboxyl of thioacetic acid and the ammonia of chitosan are improved using the mating capability of mercapto groups
Base forms amido link, and chitosan is compound with bentonite, is formed and stablizes cross-linked structure, improves the water resistance of material, present invention system
Standby molecular sieve is of low cost using bentonite as raw material, and technique is simple, and specific surface area is big, and stability is good, has stronger absorption
Ability.
Embodiment
A kind of preparation method of sulfhydryl modified active bentonite molecular sieve, it is characterised in that comprise the following steps：
（1）Activated bentonite
20 parts by weight of bentonite are put into 3 times of distilled water, are filtered after uniform stirring after static 4 decimal, by the bentonite of filtering
Ore pulp is put into drying box and dries, and adds the sulfuric acid of 40 parts by weight 60% afterwards, is placed in micro-wave oven under the conditions of 100 DEG C and heats
Filtered after 3 minutes, wash and dried after at 110 DEG C, the bentonite of drying is ground into powder with mortar, it is stand-by；
（2）It is sulfhydryl modified
By 8 parts by weight chitosans and step（1）After gained bentonite powder adds suitable water stirring and dissolving, 2-5 weight is added dropwise
Part thioacetic acid, is uniformly mixed, and adds 3 parts by weight water-soluble carbodiimides when stirring reaction 3 is small under room temperature, taking-up mixing
Solution, dialyses 3 times for 10 DEG C in lucifuge, is sealed after freeze-drying, stand-by；
（3）Prepare microballoon
By 3 parts by weight gelatin, the paraffin of 30 part by weight of liquid shapes, step is instilled with the speed of 3-6mL/min（2）In gains,
Disperse after stirring in ultrasonic cleaner, after shaping, then filtered, washed, dried 200 mesh sieve, obtains microballoon, stand-by；
（4）Crystallization
By step（3）Obtained microballoon after 30 parts by weight sodium metasilicate, 20 parts by weight lye, 10 parts by weight guiding agent for zeolite with putting into
In crystallization kettle, be heated to 100 DEG C in 35 minutes by room temperature, then heated at constant temperature be stirred at reflux 12 it is small when, naturally cool to room
Temperature filtering, filtrate are washed with deionized water, and filter, after dry filtrate, up to sulfhydryl modified active bentonite molecular sieve.
The step（1）Wash wash 3 times to neutrality with methanol, acetone, clear water successively.
The dialysis is that 5mmol/L hydrochloric acid is dialysed with 1%NaCl mixed solutions with after the dialysis once of 5mmol/L hydrochloric acid solutions
Once, then with 1mmol/L hydrochloric acid solutions dialysis twice
The pH value of the adjusting mixed solution is to use 0.5-1mol/L sodium hydroxide solutions.
The drying is one kind in low temperature drying, spray drying, vacuum drying and freeze-drying.
Claims (5)
1. a kind of preparation method of sulfhydryl modified active bentonite molecular sieve, it is characterised in that comprise the following steps：
(1) activated bentonite
20-25 parts by weight of bentonite is put into 3-5 times of distilled water, is filtered after uniform stirring after static 4-5 decimals, by filtering
Bentonite ore pulp, which is put into drying box, dries, and adds the sulfuric acid of 40-50 parts by weight 30-60% afterwards, is placed in micro-wave oven in 80-
Filtered after being heated 1-5 minutes under the conditions of 100 DEG C, wash and dried after at 100-110 DEG C, ground the bentonite of drying with mortar
It is stand-by into powdered；
(2) it is sulfhydryl modified
By 5-10 parts by weight chitosan and step（1）After gained bentonite powder adds suitable water stirring and dissolving, 2-5 weights are added dropwise
Part thioacetic acid is measured, is uniformly mixed, addition 1-4 parts by weight water-soluble carbodiimide is small after stirring reaction 2-4 under room temperature, takes out
Mixed solution, dialyses 3 times for 5-15 DEG C in lucifuge, is sealed after freeze-drying, stand-by；
(3) microballoon is prepared
By 2-5 parts by weight gelatin, the paraffin of 20-40 part by weight of liquid shapes, step is instilled with the speed of 3-6mL/min（2）Gained
In thing, disperse after stirring in ultrasonic cleaner, after shaping, then filtered, washed, dried 200 mesh sieve, obtains microballoon, treat
With；
（4）Crystallization
By step（3）Obtained microballoon is oriented to 25-40 parts by weight sodium metasilicate, 20-25 parts by weight lye, 5-13 parts by weight zeolite
Put into after agent in crystallization kettle, be heated to 90-120 DEG C in 30-40 minutes by room temperature, then to be stirred at reflux 8-24 small for heated at constant temperature
When, cooled to room temperature filtering, filtrate is washed with deionized water, and filters, after dry filtrate, up to sulfhydryl modified active bentonite
Molecular sieve.
2. according to a kind of preparation method of sulfhydryl modified active bentonite molecular sieve of claim 1, it is characterised in that the step
（1）Wash wash 3-4 times to neutrality with methanol, acetone, clear water successively.
3. according to a kind of preparation method of sulfhydryl modified active bentonite molecular sieve of claim 1, it is characterised in that the dialysis
For with after the dialysis once of 5mmol/L hydrochloric acid solutions, 5mmol/L hydrochloric acid is dialysed once with 1%NaCl mixed solutions, then uses 1mmol/L
Hydrochloric acid solution is dialysed twice.
4. according to a kind of preparation method of sulfhydryl modified active bentonite molecular sieve of claim 1, it is characterised in that the tune
The pH value for saving mixed solution is to use 0.5-1mol/L sodium hydroxide solutions.
5. according to a kind of preparation method of sulfhydryl modified active bentonite molecular sieve of claim 1, it is characterised in that described is dry
Dry is one kind in low temperature drying, spray drying, vacuum drying and freeze-drying.
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| CN201711061431.9A CN108014754A (en) | 2017-11-02 | 2017-11-02 | A kind of preparation method of sulfhydryl modified active bentonite molecular sieve |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020156291A1 (en) * | 2019-01-30 | 2020-08-06 | 福州大学 | Physical and chemical double cross-linked network high-strength gelatin hydrogel and preparation method therefor |
| CN113100086A (en) * | 2021-04-22 | 2021-07-13 | 铜陵博锋实业有限公司 | Zeolite cat litter and production process thereof |
| CN115072851A (en) * | 2022-08-19 | 2022-09-20 | 山东诺尔生物科技有限公司 | Landfill leachate treating agent and preparation method thereof |
| CN117256487A (en) * | 2023-09-11 | 2023-12-22 | 山东辛化硅胶有限公司 | Easily-treated water-soluble cat litter and preparation method thereof |
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| CN101580245A (en) * | 2009-05-31 | 2009-11-18 | 苏州中材非金属矿工业设计研究院有限公司 | Method for preparing active floridin through microwave activation |
| CN104014315A (en) * | 2014-06-06 | 2014-09-03 | 黄淮学院 | Sulfydryl-phenyl thiosemicarbazide chitosan modified zeolite as well as preparation and applications thereof |
| CN104511296A (en) * | 2013-09-26 | 2015-04-15 | 湖南理工学院 | Porous molecular sieve composite material and preparation method thereof |
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2017
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Patent Citations (3)
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| CN101580245A (en) * | 2009-05-31 | 2009-11-18 | 苏州中材非金属矿工业设计研究院有限公司 | Method for preparing active floridin through microwave activation |
| CN104511296A (en) * | 2013-09-26 | 2015-04-15 | 湖南理工学院 | Porous molecular sieve composite material and preparation method thereof |
| CN104014315A (en) * | 2014-06-06 | 2014-09-03 | 黄淮学院 | Sulfydryl-phenyl thiosemicarbazide chitosan modified zeolite as well as preparation and applications thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020156291A1 (en) * | 2019-01-30 | 2020-08-06 | 福州大学 | Physical and chemical double cross-linked network high-strength gelatin hydrogel and preparation method therefor |
| CN113100086A (en) * | 2021-04-22 | 2021-07-13 | 铜陵博锋实业有限公司 | Zeolite cat litter and production process thereof |
| CN115072851A (en) * | 2022-08-19 | 2022-09-20 | 山东诺尔生物科技有限公司 | Landfill leachate treating agent and preparation method thereof |
| CN115072851B (en) * | 2022-08-19 | 2022-11-11 | 山东诺尔生物科技有限公司 | Landfill leachate treating agent and preparation method thereof |
| CN117256487A (en) * | 2023-09-11 | 2023-12-22 | 山东辛化硅胶有限公司 | Easily-treated water-soluble cat litter and preparation method thereof |
| CN117256487B (en) * | 2023-09-11 | 2024-03-26 | 山东辛化硅胶有限公司 | Easily-treated water-soluble cat litter and preparation method thereof |
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