CN108014753A - A kind of preparation method of porous modified alta-mud granule adsorbent - Google Patents
A kind of preparation method of porous modified alta-mud granule adsorbent Download PDFInfo
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- CN108014753A CN108014753A CN201711061368.9A CN201711061368A CN108014753A CN 108014753 A CN108014753 A CN 108014753A CN 201711061368 A CN201711061368 A CN 201711061368A CN 108014753 A CN108014753 A CN 108014753A
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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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Abstract
The invention discloses a kind of preparation method of porous modified alta-mud granule adsorbent, after sodium-ionized bentonite being carried out by sodium chloride, after sulfuric acid activated bentonite, after iron chloride is soaked using acid afterwards, then poly- iron carbonyl chitosan is made with sodium hydroxide and chitosan reaction, bentonite after activation and poly- iron carbonyl chitosan are subjected to reaction and carry out intercalation, is finally prepared by mixing into particle with flake asbestos, straw powder, both porous modified alta-mud granule adsorbent.Granule adsorbent prepared by the present invention is of low cost, high selectivity, and stability is good, adsorbs long lifespan, renewable.
Description
Technical field
The invention belongs to bentonite processing technique field, and in particular to a kind of system of porous modified alta-mud granule adsorbent
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.
Asbestos are the general terms of the silicoide of natural fiber, are a kind of silicates for being widely used in building materials fire-proof plate
Class mineral fibres, and unique natural mineral fiber.The characteristics of asbestos fibre is heat-resisting, non-ignitable, water-fast, acidproof, chemically-resistant
Corrosion, and since force intensity and internal surface area are big, therefore have very big adsorption capacity.
The content of the invention
The present invention provides a kind of preparation method of porous modified alta-mud granule adsorbent, granular absorption prepared by the present invention
Agent is of low cost, high selectivity, and stability is good, adsorbs long lifespan, renewable.
The present invention is achieved by the following technical solutions：
A kind of preparation method of porous modified alta-mud granule adsorbent, it is characterised in that comprise the following steps：
（1）Activate sodium-ionized 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 take add 2-5 parts by wt NaCl, when heating stirring 1-3 is small under the conditions of 60-90 DEG C after, filtering rear slurry put
Enter in drying box and dry, add the sulfuric acid of 40-50 parts by weight 30-60% afterwards, 80-100 DEG C heat 1-2 it is small when after filter,
Washing is dried after at 100-110 DEG C, and the bentonite of drying is ground into powder with mortar, stand-by；
（2）Modified chlorinated iron
5-10 parts by weight iron chloride is added in suitable hydrochloric acid solution soak 1-2 it is small when after, 15-25 weights are slowly added to after filtering
Part water is measured, the sodium hydroxide of 1-5 parts by weight, when ball milling mixing 5-8 is small, adds 0.1-0.3 parts by weight chitosans, under nitrogen protection
Be stirred at room temperature 4-8 it is small when, it is stand-by；
（3）Intercalation
By step（1）Gained powder adds suitable water to be made into suspension, and in the case where 55-65 DEG C is stirred continuously, step is slowly added dropwise（2）
Resulting solution, is placed in micro-wave oven under the conditions of 60-80 DEG C after heating 1-60 minutes and filters, wash and dried after at 100-110 DEG C
It is dry, it is ground into powder, it is stand-by；
（4）Shaping
By step（3）Material mixed with 5-8 parts by weight flake asbestos, 5-10 parts by weight straw powders add 10% water, be placed in ultrasound
In ripple washer disperse, dried using drying and crushing after cooked flake wrapping machine extrusion forming, both porous modified alta-mud granule adsorbent.
The step（1）Wash wash 3-4 times to neutrality with methanol, acetone, clear water successively.
The concentration of sodium hydroxide solution is 0.5-1mol/L, concentration of hydrochloric acid solution 0.5-1mol/L, sulfuric acid solution
Concentration is 0.5-1mol/L.
The step（2）Particle mean size after middle ball milling reaches 0.8-3 microns.
Described crushing drying is that it is 1-4mm to be crushed to granularity using dryer, be dried to moisture 10% with
Under.
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 carries out sodium-ionized bentonite by sodium chloride, after sulfuric acid activated bentonite, iron chloride is used into acid afterwards
After being soaked, poly- iron carbonyl-chitosan is then made with sodium hydroxide and chitosan reaction, by the bentonite after activation with gathering
Iron carbonyl-chitosan carry out reaction carry out intercalation, be finally prepared by mixing into particle with flake asbestos, straw powder, both porous modification
Bentonite clay particle adsorbent.Sodium-ionized bentonite is carried out after purification, bentonitic cation exchange capacity is substantially better than original soil, more has
Beneficial to intercalation modifying is carried out, after acidifying, its structure can be destroyed, improves the reactivity of raw material, the hydrogen-oxygen of sodium hydroxide in water
Radical ion is polymerize with iron ion so that condensate increases, and after addition chitosan is crosslinked, stable system, carries out intercalation
After bentonite, the catalysis of intercalation compound bentonite is adjusted, change bentonite interfloor distance, removing absorption water, changes
Its traffic micro-simulation, can strengthen its adsorption capacity, and the addition of flake asbestos, straw powder make it that absorbent particles appearance is porous, carries
High-specific surface area and adsorption capacity.Granule adsorbent prepared by the present invention is of low cost, high selectivity, and stability is good, adsorbs the service life
It is long, it is renewable.
Embodiment
A kind of preparation method of porous modified alta-mud granule adsorbent, it is characterised in that comprise the following steps：
（1）Activate sodium-ionized bentonite
20 parts by weight of bentonite are put into 4 times of distilled water, are filtered after uniform stirring after static 5 decimal, by the bentonite of filtering
Ore pulp, which takes, adds 3 parts by wt NaCl, when heating stirring 2 is small under the conditions of 80 DEG C after, filtering rear slurry is put into drying box and dries
It is dry, add the sulfuric acid of 45 parts by weight 30-60% afterwards, when 90 DEG C of heating 1.5 are small after filter, wash and dried after at 100 DEG C,
The bentonite of drying is ground into powder with mortar, it is stand-by；
（2）Modified chlorinated iron
After when immersion 1.5 is small in the suitable hydrochloric acid solution of 8 parts by weight iron chloride addition, 20 parts by weight are slowly added to after filtering
Water, the sodium hydroxide of 4 parts by weight, when ball milling mixing 6 is small, adds 0.2 parts by weight chitosan, it is small to be stirred at room temperature 5 under nitrogen protection
When, it is stand-by；
（3）Intercalation
By step（1）Gained powder adds suitable water to be made into suspension, and in the case where 60 DEG C are stirred continuously, step is slowly added dropwise（2）Institute
Solution is obtained, is placed in micro-wave oven under the conditions of 70 DEG C after heating 30 minutes and filters, wash and dried after at 100 DEG C, pulverized
Last shape, it is stand-by；
（4）Shaping
By step（3）Material mixed with 6 parts by weight flake asbestos, 8 parts by weight straw powders add 10% water, be placed in ultrasonic cleaning
In device disperse, dried using drying and crushing after cooked flake wrapping machine extrusion forming, both porous modified alta-mud granule adsorbent.
The step（1）Wash wash 3 times to neutrality with methanol, acetone, clear water successively.
The concentration of sodium hydroxide solution is 0.5-1mol/L, concentration of hydrochloric acid solution 0.5-1mol/L, sulfuric acid solution
Concentration is 0.5-1mol/L.
The step（2）Particle mean size after middle ball milling reaches 0.8-3 microns.
Described crushing drying is that it is 1-4mm to be crushed to granularity using dryer, be dried to moisture 10% with
Under.
The drying is one kind in low temperature drying, spray drying, vacuum drying and freeze-drying.
Claims (6)
1. a kind of preparation method of porous modified alta-mud granule adsorbent, it is characterised in that comprise the following steps：
（1）Activate sodium-ionized 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 take add 2-5 parts by wt NaCl, when heating stirring 1-3 is small under the conditions of 60-90 DEG C after, filtering rear slurry put
Enter in drying box and dry, add the sulfuric acid of 40-50 parts by weight 30-60% afterwards, 80-100 DEG C heat 1-2 it is small when after filter,
Washing is dried after at 100-110 DEG C, and the bentonite of drying is ground into powder with mortar, stand-by；
（2）Modified chlorinated iron
5-10 parts by weight iron chloride is added in suitable hydrochloric acid solution soak 1-2 it is small when after, 15-25 weights are slowly added to after filtering
Part water is measured, the sodium hydroxide of 1-5 parts by weight, when ball milling mixing 5-8 is small, adds 0.1-0.3 parts by weight chitosans, under nitrogen protection
Be stirred at room temperature 4-8 it is small when, it is stand-by；
（3）Intercalation
By step（1）Gained powder adds suitable water to be made into suspension, and in the case where 55-65 DEG C is stirred continuously, step is slowly added dropwise（2）
Resulting solution, is placed in micro-wave oven under the conditions of 60-80 DEG C after heating 1-60 minutes and filters, wash and dried after at 100-110 DEG C
It is dry, it is ground into powder, it is stand-by；
（4）Shaping
By step（3）Material mixed with 5-8 parts by weight flake asbestos, 5-10 parts by weight straw powders add 10% water, be placed in ultrasound
In ripple washer disperse, dried using drying and crushing after cooked flake wrapping machine extrusion forming, both porous modified alta-mud granule adsorbent.
2. according to a kind of preparation method of porous modified alta-mud granule adsorbent 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 porous modified alta-mud granule adsorbent of claim 1, it is characterised in that the hydrogen
Sodium hydroxide solution concentration is 0.5-1mol/L, concentration of hydrochloric acid solution 0.5-1mol/L, sulfuric acid solution concentration are 0.5-1mol/L.
4. according to a kind of preparation method of porous modified alta-mud granule adsorbent of claim 1, it is characterised in that the step
Suddenly（2）Particle mean size after middle ball milling reaches 0.8-3 microns.
5. according to a kind of preparation method of porous modified alta-mud granule adsorbent of claim 1, it is characterised in that the powder
Broken drying is that it is 1-4mm to be crushed to granularity, is dried to moisture below 10% using dryer.
6. according to a kind of preparation method of porous modified alta-mud granule adsorbent 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108867148A (en) * | 2018-08-07 | 2018-11-23 | 枣庄市天龙纸业有限公司 | A kind of low basis weight decorating printing paper and preparation method thereof |
| CN109022089A (en) * | 2018-08-21 | 2018-12-18 | 芜湖聚焰生物质能源科技有限公司 | A kind of method of swollen soft straws used for preparing fuel |
| CN110075786A (en) * | 2019-04-04 | 2019-08-02 | 深圳清纳科技有限公司 | The method that activated clay is prepared using ultrasound enhancing activation method |
| CN114755195A (en) * | 2022-06-14 | 2022-07-15 | 浙江省立同德医院(浙江省精神卫生研究院) | Preparation method of reagent for quickly detecting urine protein |
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| CN103191582A (en) * | 2013-03-26 | 2013-07-10 | 太原理工大学 | Method for removing bivalent copper ions in aqueous solution |
| CN104841396A (en) * | 2015-04-22 | 2015-08-19 | 马鞍山市顺达环保设备有限公司 | Acid-resistant adsorbent prepared from straw and bentonite and preparation method thereof |
| CN106865560A (en) * | 2016-12-22 | 2017-06-20 | 芜湖恒杰膨润土科技有限公司 | A kind of sodium-ionized bentonite production technology |
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| CN103191582A (en) * | 2013-03-26 | 2013-07-10 | 太原理工大学 | Method for removing bivalent copper ions in aqueous solution |
| CN104841396A (en) * | 2015-04-22 | 2015-08-19 | 马鞍山市顺达环保设备有限公司 | Acid-resistant adsorbent prepared from straw and bentonite and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108867148A (en) * | 2018-08-07 | 2018-11-23 | 枣庄市天龙纸业有限公司 | A kind of low basis weight decorating printing paper and preparation method thereof |
| CN109022089A (en) * | 2018-08-21 | 2018-12-18 | 芜湖聚焰生物质能源科技有限公司 | A kind of method of swollen soft straws used for preparing fuel |
| CN110075786A (en) * | 2019-04-04 | 2019-08-02 | 深圳清纳科技有限公司 | The method that activated clay is prepared using ultrasound enhancing activation method |
| CN114755195A (en) * | 2022-06-14 | 2022-07-15 | 浙江省立同德医院(浙江省精神卫生研究院) | Preparation method of reagent for quickly detecting urine protein |
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