CN107126934A - A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres - Google Patents
A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres Download PDFInfo
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- CN107126934A CN107126934A CN201710570859.XA CN201710570859A CN107126934A CN 107126934 A CN107126934 A CN 107126934A CN 201710570859 A CN201710570859 A CN 201710570859A CN 107126934 A CN107126934 A CN 107126934A
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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
- B01J20/22—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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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
- B01J20/02—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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/02—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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- 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
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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Abstract
The invention discloses the preparation method that a kind of borax cooperates with silica modified lobster shell adsorption microspheres, using lobster shell after high-pressure steam sterilizing pan carries out high-temperature process, then add after being soaked in sodium hydroxide solution after squeezing crushing, it is then dissolved in ethanol, after addition silica is modified with borax afterwards, add bentonite, alkali is added after long agitation to be reacted with epoxychloropropane, afterwards and paraffin, both obtained after the shaping of emulsifying agent mixing dispersion and emulsion, adsorption microspheres preparation technology of the present invention is simple, the quick harmful substance for catching and adsorbing, it is with low cost, stability is good, the big advantage of adsorption capacity.
Description
Technical field
The invention belongs to adsorption microspheres technical field, and in particular to a kind of borax cooperates with silica modified lobster shell absorption
The preparation method of microballoon.
Background technology
China cray industry is developed rapidly in recent years, while national material life is met, is also generated substantial amounts of
Using shrimp shell as the discarded object of representative.Chitin is natural high as obtained from shrimp, crab or insect shell pass through soda acid working process
Molecular material, and chitosan is the derivative of chitin.
Chitin, also known as chitin, chitin, chitin etc., are by 2-Acetamido-2-deoxy-D-glucose polycondensation
Linear polymer.Its close crystal structure makes its water insoluble, diluted acid, alkali, alcohol and other organic solvents.This
Its application is limited to a certain extent.But its deacetylation product chitosan, due to adding active group-ammonia
Base, makes its dissolubility make moderate progress, and application for chitin compared with also having obtained greatly promoting.During chitosan is nature
Content in unique alkaline polysaccharide, nature is only second to cellulose.
Therefore, chitosan-based compound bio sorbing material is prepared using accessory substance-shrimp shell of cray, can be achieved to become
Waste be changed into values, twice laid, embodies the theory of recycling economy.
The content of the invention
The object of the invention is exactly that defect not thorough in order to make up absorption, non-renewable cooperates with dioxy there is provided a kind of borax
SiClx is modified the preparation method of lobster shell adsorption microspheres, what adsorption microspheres preparation technology of the present invention simply, quickly caught and adsorbed
Harmful substance, with low cost, stability is good, the big advantage of adsorption capacity.
The present invention is achieved by the following technical solutions：
A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres, comprises the following steps：
（1）20-30 parts by weight lobster shells are placed in high-pressure steam sterilizing pan 120-130 DEG C of temperature, insulation 5-10 minutes are set
Afterwards, after taking-up addition 50-80 parts by weight 0.1-0.5mol/L sodium hydrate aqueous solutions soak 12-24 hours at 20-25 DEG C, clearly
Water washing 3-4 times, dries, and squeezer carries out pulverization process, stand-by；
（2）By step（1）Gains are dissolved in 100-150 parts by weight of ethanol, are added 5-8 parts by weight of silica and are well mixed
Afterwards, it is slowly added to 2-6 parts by weight boraxs under agitation, ultrasonic reaction 0.5-1.5 hours, suction filtration after cooling, and with anhydrous
Ethanol washs 2-4 times, 40-50 DEG C after dry 12-24 hours, stand-by；
（3）By step（2）Gains add 5-10 parts by weight of bentonite, after stirring at low speed 12-24 hours, add 150-
200 parts by weight of sodium hydroxide solution, add 7-8 parts by weight epoxy chloropropanes, after 60-70 DEG C of continuous high speed is stirred 2-4 hours,
By suction filtration, clear water is washed 3-4 times, and 40-50 DEG C dry 12-24 hours, and grinding is stand-by；
（4）By step（3）Gains, which are added in 30-50 parts by weight acetic acid solutions, to be dissolved, and adds 20-40 part by weight of liquid shapes
0.05-0.15 parts by weight Emulsifier is added dropwise after 5-15 minute in paraffin, 50-60 DEG C of stirring, and stirring lower insulation emulsification 5-15 minutes is super
After disperseing in sound wave washer, being molded, then carry out suction filtration, washing, 40-50 DEG C after drys 12-24 hours both the borax is assisted
With silica modified lobster shell adsorption microspheres.
Described squeezing and crushing is carried out on squeezing pulverizer, between the bottom squeezing roller of squeezing pulverizer and top squeeze roller
Carry out.
The described borax that is slowly added to is that magnetic agitation heating in 2-6 parts by weight borax addition 20-30 parts by weight water is molten
Solution, then solution is added dropwise, rate of addition is 2-3ml/min.
The described step（3）Middle emulsifying agent is span-80.
Described step（4）In washing to carry out with methanol, acetone washing 3-4 times successively.
It is an advantage of the invention that：
（1）The present invention after high-pressure steam sterilizing pan carries out high-temperature process, then adds sodium hydroxide first with lobster shell
After squeezing is crushed after being soaked in solution, it is then dissolved in ethanol, after addition silica is modified with borax afterwards, adds
Bentonite, after long agitation add alkali is reacted with epoxychloropropane, and afterwards and paraffin, emulsifying agent mixing disperses newborn
Both obtained after chemical conversion type.Lobster shell passes through in high-pressure steam sterilizing pan sterilization treatment, loose shrimp shell, alkali lye can accelerate lobster after immersion
The rate of dissolution of protein in shell, sloughs part second phthalidyl, long-chain is broken after squeezing is crushed, short chain increase, in ethanol
With borax hydrolysis occurs for chitin after dissolving, and dehydration esterification generates borax ester bond, forms stable cross-linked structure, can
By heavy metal ion catch the water resistance that material is also improved with adsorbing.
（2）Adsorption microspheres preparation technology of the present invention is simple, the quick harmful substance for catching and adsorbing, with low cost, stable
Good, the big advantage of adsorption capacity of property.
Embodiment
A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres, comprises the following steps：
（1）After being placed in 125 DEG C of temperature of setting in high-pressure steam sterilizing pan by 25 parts by weight lobster shells, be incubated 8 minutes, take out and add
After 70 parts by weight 0.3mol/L sodium hydrate aqueous solutions soak 18 hours at 23 DEG C, clear water is washed 3 times, is dried, squeezer enters
Row pulverization process, it is stand-by；
（2）By step（1）Gains are dissolved in 120 parts by weight of ethanol, after 6 parts by weight of silica of addition are well mixed, are being stirred
4 parts by weight boraxs, ultrasonic reaction 1 hour, suction filtration after cooling are slowly added under the conditions of mixing, and is washed 3 times, 45 DEG C with absolute ethyl alcohol
It is stand-by after drying 18 hours；
（3）By step（2）Gains add 8 parts by weight of bentonite, after stirring at low speed 18 hours, add 180 parts by weight hydrogen
Sodium hydroxide solution, adds 7.5 parts by weight epoxy chloropropanes, after 65 DEG C of continuous high speeds are stirred 3 hours, by suction filtration, clear water is washed
Wash 3 times, 45 DEG C of dryings 18 hours, grinding is stand-by；
（4）By step（3）Gains, which are added in 30-50 parts by weight acetic acid solutions, to be dissolved, and adds the stone of 30 part by weight of liquid shapes
0.1 parts by weight Emulsifier is added dropwise after 10 minutes in wax, 55 DEG C of stirrings, the lower insulation emulsification of stirring 10 minutes, in ultrasonic cleaner point
Dissipate, after shaping, then carry out suction filtration, washing, after 45 DEG C of drying 18 hours both the silica modified lobster shell of the borax collaboration
Adsorption microspheres.
Described squeezing and crushing is carried out on squeezing pulverizer, between the bottom squeezing roller of squeezing pulverizer and top squeeze roller
Carry out.
The described borax that is slowly added to is that 4 parts by weight boraxs are added into magnetic agitation in 25 parts by weight water to dissolve by heating, then
Solution is added dropwise, rate of addition is 1.5ml/min.
The described step（3）Middle emulsifying agent is span-80.
Described step（4）In washing to carry out with methanol, acetone washing 3 times successively.
Claims (5)
1. a kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres, it is characterised in that including following step
Suddenly：
After being placed in 120-130 DEG C of temperature of setting in high-pressure steam sterilizing pan by 20-30 parts by weight lobster shells, be incubated 5-10 minutes,
After taking-up addition 50-80 parts by weight 0.1-0.5mol/L sodium hydrate aqueous solutions soak 12-24 hours at 20-25 DEG C, clear water
Washing 3-4 times, dries, and squeezer carries out pulverization process, stand-by；
By step（1）Gains are dissolved in 100-150 parts by weight of ethanol, after addition 5-8 parts by weight of silica is well mixed,
2-6 parts by weight boraxs, ultrasonic reaction 0.5-1.5 hours, suction filtration after cooling are slowly added under stirring condition, and is washed with absolute ethyl alcohol
Wash 2-4 times, 40-50 DEG C after dry 12-24 hours, it is stand-by；
By step（2）Gains add 5-10 parts by weight of bentonite, after stirring at low speed 12-24 hours, add 150-200 weights
Part sodium hydroxide solution is measured, 7-8 parts by weight epoxy chloropropanes is added, after 60-70 DEG C of continuous high speed is stirred 2-4 hours, passes through
Suction filtration, clear water is washed 3-4 times, and 40-50 DEG C dry 12-24 hours, grinding, stand-by；
By step（3）Gains, which are added in 30-50 parts by weight acetic acid solutions, to be dissolved, and adds the stone of 20-40 part by weight of liquid shapes
0.05-0.15 parts by weight Emulsifier is added dropwise after 5-15 minute in wax, 50-60 DEG C of stirring, and stirring lower insulation emulsification 5-15 minutes is ultrasonic
After disperseing in ripple washer, being molded, then carry out suction filtration, washing, 40-50 DEG C after drys 12-24 hours both the borax is cooperateed with
Silica modified lobster shell adsorption microspheres.
2. cooperateing with the preparation method of silica modified lobster shell adsorption microspheres according to a kind of borax of claim 1, its feature exists
In described squeezing and crushing is carried out on squeezing pulverizer, is carried out between the bottom squeezing roller of squeezing pulverizer and top squeeze roller.
3. cooperateing with the preparation method of silica modified lobster shell adsorption microspheres according to a kind of borax of claim 1, its feature exists
In, the described borax that is slowly added to is that 2-6 parts by weight borax is added into magnetic agitation in 20-30 parts by weight water to dissolve by heating, then
Solution is added dropwise, rate of addition is 2-3ml/min.
4. cooperateing with the preparation method of silica modified lobster shell adsorption microspheres according to a kind of borax of claim 1, its feature exists
In the described step（3）Middle emulsifying agent is span-80.
5. cooperateing with the preparation method of silica modified lobster shell adsorption microspheres according to a kind of borax of claim 1, its feature exists
In described step（4）In washing to carry out with methanol, acetone washing 3-4 times successively.
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| CN201710570859.XA CN107126934A (en) | 2017-07-13 | 2017-07-13 | A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres |
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| CN201710570859.XA CN107126934A (en) | 2017-07-13 | 2017-07-13 | A kind of borax cooperates with the preparation method of silica modified lobster shell adsorption microspheres |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111271A (en) * | 2013-03-04 | 2013-05-22 | 福州大学 | Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent |
| CN103495394A (en) * | 2013-08-30 | 2014-01-08 | 蚌埠首创滤清器有限公司 | Modified activated carbon for removing organic pollutants and its preparation method |
| CN105032372A (en) * | 2015-09-11 | 2015-11-11 | 江苏振宇环保科技有限公司 | Method for preparing chitosan-bentonite adsorbing material prepared from shrimp shells |
| CN105126773A (en) * | 2015-08-21 | 2015-12-09 | 中国科学院南海海洋研究所 | Renewable heavy metal adsorption material with shrimp and crab shells as raw material, and preparation method, regeneration method and application thereof |
-
2017
- 2017-07-13 CN CN201710570859.XA patent/CN107126934A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111271A (en) * | 2013-03-04 | 2013-05-22 | 福州大学 | Preparation method of chitosan-grafted beta-cyclodextrin bonded silica gel absorbent |
| CN103495394A (en) * | 2013-08-30 | 2014-01-08 | 蚌埠首创滤清器有限公司 | Modified activated carbon for removing organic pollutants and its preparation method |
| CN105126773A (en) * | 2015-08-21 | 2015-12-09 | 中国科学院南海海洋研究所 | Renewable heavy metal adsorption material with shrimp and crab shells as raw material, and preparation method, regeneration method and application thereof |
| CN105032372A (en) * | 2015-09-11 | 2015-11-11 | 江苏振宇环保科技有限公司 | Method for preparing chitosan-bentonite adsorbing material prepared from shrimp shells |
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