CN106237991B - A kind of adsorbent and its preparation method and application - Google Patents
A kind of adsorbent and its preparation method and application Download PDFInfo
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- CN106237991B CN106237991B CN201610695138.7A CN201610695138A CN106237991B CN 106237991 B CN106237991 B CN 106237991B CN 201610695138 A CN201610695138 A CN 201610695138A CN 106237991 B CN106237991 B CN 106237991B
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/203—Iron or iron compound
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Abstract
The present invention relates to a kind of adsorbents and its preparation method and application, belong to organic high molecular compound technical field.The adsorbent is a kind of mixture, and main component includes the substances such as a kind of high-molecular chelating agent, modification of chitosan, polyacrylamide and sodium metaaluminate.Adsorbent synthesized by the application is used for high performance water-reducer field, it can be by Ca in water2+、Mg2+Total content is lower than 0.3mg/L, Zn2+、Fe2+Total content is lower than 0.05mg/L.
Description
Technical field
The present invention relates to a kind of adsorbents and its preparation method and application, belong to organic high molecular compound technical field.
Background technique
In recent years, with the fast development of concrete technology and building trade, the demand of polycarboxylate water-reducer constantly increases
Greatly, the synthesis process of polycarboxylate water-reducer belongs to Raolical polymerizable, needs a large amount of water as solvent in reaction process, but not
Contain a small amount of Ca in the industrial water of processing2+、Mg2+、Fe2+、Zn2+Plasma, Ca2+、Mg2+Ion is easily made with reactive component
With generation insoluble salt has certain inhibition, Zn2+、Fe2+Plasma has reproducibility, easily to the oxidation-of polymerization reaction
Reduction initiating system generation effect, causes free radical number to reduce, and seriously affects the quality of synthesis water-reducing agent, adds product color
It is deep.
In high performance water-reducer technique common water be through ion-exchange treated industrial water, using specific sun from
Sub-exchange resin is cemented out the calcium and magnesium plasma in water with sodium ion, reduces influence of the calcium and magnesium plasma to synthetic reaction,
But still contain a certain amount of Ca in this method treated industry water2+、Mg2+、Fe2+、Zn2+Ion cannot be completely eliminated it to poly-
The influence of reaction is closed, to overcome disadvantages mentioned above, the present invention provides a kind of adsorbents, use water by adsorption precipitation removal synthesis
In remaining Ca2+、Mg2+、Fe2+、Zn2+Ion reduces its content to trace level, eliminates to polycarboxylate water-reducer synthetic reaction
Influence.
Based on this, the application is made.
Summary of the invention
Present invention firstly provides a kind of preparation methods of adsorbent, for removing in high performance water-reducer process water
Ca2+、Mg2+、Zn2+、Fe2+Plasma eliminates its influence to high performance water-reducer reaction, and adsorbent production is simple, user
Just, have the characteristics that quick, efficient.
The adsorbent is a kind of mixture, and main component includes a kind of high-molecular chelating agent, modification of chitosan, polyacrylamide
The substances such as amine and sodium metaaluminate, specific preparation method are as follows：
(1) it weighs a certain amount of Isosorbide-5-Nitrae butanediamine to be dissolved in dehydrated alcohol, heating water bath is to 40-60 DEG C, alcohol reflux shape
Under state, a certain amount of Bi-phenolic Methan e epoxy resin is added, feed intake point 3 progress, after feeding intake, keeps temperature-resistant stirring
30-60min obtains intermediate product solution A；
(2) it weighs in a certain amount of sodium phosphite investment solution A, is warming up to 40-60 DEG C, is stirred at reflux under state, be added dropwise
10% carbon disulfide ethanol solution, insulation reaction 1-4h after completion of dropwise addition add a certain amount of sodium hydrate solid, stirring
After 5-30 minutes, alcohol solvent and small-molecule substance in product are sloughed in vacuum distillation, and vacuum is dry at 45-55 DEG C of resultant product
It is dry to get high-molecular chelating agent.
(3) it is weighed in each component investment flask by following parts by weight, a small amount of water is added under room temperature and is mixed evenly,
It pours into mold and is dried in vacuo to get product adsorbent,
Further, as preferred：
The average molecular weight of the chelating agent is 1200~1500g/mol.
The average molecular weight of the Bi-phenolic Methan e epoxy resin is 514g/mol, Bi-phenolic Methan e epoxy resin and Isosorbide-5-Nitrae
The molar ratio of butanediamine is (2-2.5)：1, hybrid reaction temperature is 50-55 DEG C.
The molar ratio of the sodium phosphite and Isosorbide-5-Nitrae butanediamine is (1-1.5)：1, mole of carbon disulfide and Isosorbide-5-Nitrae butanediamine
Than being (1-1.5):1.
The time for adding of the carbon disulfide ethanol solution is 2.5-3h, and drip reacting temperature is 60-70 DEG C, soaking time
2h。
The modification of chitosan is through monoxone and the modified carboxymethyl chitosan powder of sodium hydroxide, with Isosorbide-5-Nitrae fourth
The molar ratio of diamines is 1-2.5：1.
Its structural formula of adsorbent prepared by the application is：
Adsorbent synthesized by the application is used for high performance water-reducer field, is used in water for removing synthesis technology
Ca2+、Mg2+、Fe2+、Zn2+When ion, the dosage of adsorbent is not less than 0.5g/L, preferably 0.5-0.8g/L, by Ca in water2+、
Mg2+Total content is lower than 0.3mg/L, Zn2+、Fe2+Total content is lower than 0.05mg/L.
Using adsorbent treated hydration at polycarboxylate water-reducer product, compared with untreated water sintetics,
Flowing degree of net paste of cement improves 45mm or more, and after room temperature 7 days, 120 or more product color value difference, adsorbent can be significant
Promote the quality of sintetics.
Detailed description of the invention
Ca in water after the processing of Fig. 1 difference adsorbent amount2+、Mg2+Total content；
Fig. 2 is Zn in water after the processing of different adsorbent amounts2+、Fe2+Total content.
Specific embodiment
Patent is further elaborated below in conjunction with specific embodiment.
Embodiment 1：The adsorbent prepared under different process
It weighs Isosorbide-5-Nitrae butanediamine and Bi-phenolic Methan e epoxy resin puts into and blender is housed, the four of thermometer and reflux unit
In mouth flask, ethyl alcohol does heating in water bath for reaction under conditions of solvent, and Bi-phenolic Methan e epoxy resin, which divides 3 times, to feed intake, control reaction
Temperature is 55 DEG C, insulated and stirred 1h after feeding intake.In the reaction solution for weighing a certain amount of phosphorous acid investment again, warming-in-water is extremely
65 DEG C, under alcohol reflux state, 10% carbon disulfide ethanol solution, time for adding 3h, after completion of dropwise addition are added dropwise while stirring
Insulation reaction 2h adds a small amount of sodium hydrate solid, and the alcohol solvent in reaction solution is sloughed in vacuum distillation after ten minutes for stirring
And small-molecule substance, vacuum drying presses table 1 to get high-molecular chelating agent, the mol ratio of reaction mass at 50 DEG C of resultant product
Shown in the ratio of middle chelating agent preparation experiment 1.
The chelating agent of preparation, chitosan, polyacrylamide, sodium metaaluminate are pressed into quality proportioning 5：3：2：1 weighs, and puts into
In round-bottomed flask, a small amount of water is added under room temperature and is mixed evenly, pours into mold and is dried in vacuo, obtains adsorbent product, such as
Number is A1 shown in table 1.
Based on the preparation process of adsorbent A 1, the molar ratio of reaction mass in chelating agent preparation is adjusted according to table 1, is synchronised
The chelating agent of different molecular weight, and example chelating agent in mass ratio are prepared under rapid：Chitosan：Polyacrylamide：Sodium metaaluminate=5：
3：2：1 weighs each component, is mixed evenly after a small amount of water is added, and adsorbent is made after vacuum drying, and number is as shown in table 1,
Respectively A2, A3, A4, A5.
The molar ratio of reaction mass in the preparation experiment of 1 chelating agent of table
Embodiment 2：Adsorption effect of the adsorbent of different process index to water intermediate ion
Adsorbent A 1, A2, A3, A4, A5 are studied to Ca in water2+、Mg2+、Zn2+、Fe2+The adsorption effect of ion.Measure six parts
1L polycarboxylate water-reducer synthesis water, number 1-6 is spare, weighs 0.4g adsorbent A 1-A5 respectively, and the diminishing of number 1-5 is added
With in water, adsorbent is not added as blank group in number 6 for agent synthesis, is stood after stirring 1h under room temperature, is deposited in test water
The precipitating time completely used.The completely rear filtering of precipitating, using the Ca of Atomic Absorption Spectrometry amount filtrate2+、Mg2+、Zn2+、
Fe2+Ion concentration, each sample measurement are averaged three times, and data record is as shown in table 2.
The ion concentration of water and precipitating complete time after the processing of 2 adsorbent of table
In conjunction with Tables 1 and 2 it is found that the chelating agent of different material proportion preparation has a great impact to the performance of adsorbent,
The ion concentration of water has notable difference after adsorbent A 1, A2, A3, A4, A5 processing, and the deposition rate of adsorbent is not also identical, main
It wants the reason is that in the preparation process of chelating agent, Bi-phenolic Methan e epoxy resin influences the deposition rate of the adsorbent of preparation,
It reacts dosage to increase, chelator molecule amount increases, and the sorbent deposition rate of preparation is accelerated, and when deposition rate is too fast, then adsorbs
Agent weakens the adsorption capacity of water intermediate ion.Sodium phosphite plays Ca in absorption water2+、Mg2+The effect of ion, carbon disulfide master
Adsorb the Zn in water2+、Fe2+Ion increases the reaction dosage of the two, can accelerate adsorbent to the absorption speed of water intermediate ion
Rate, but when dosage is excessive, easily leads to that chelator molecule amount is excessive, and the sorbent deposition rate finally prepared is too fast, is unfavorable in water
The Adsorption of ion.It being comprehensively compared, the adsorption effect of adsorbent A 5 is more excellent, the material proportion of preparation experiment 5 in table 1 is selected,
The chelating agent of preparation has preferable adsorption effect.
The quality proportioning for changing chelating agent, chitosan, polyacrylamide, sodium metaaluminate compares the adsorbent of preparation to subtracting
Ca in aqua synthesis water2+、Mg2+、Zn2+、Fe2+The adsorption effect of ion.
Embodiment 3：The adsorbent prepared under different process
It weighs Isosorbide-5-Nitrae butanediamine and Bi-phenolic Methan e epoxy resin puts into and blender is housed, the four of thermometer and reflux unit
In mouth flask, ethyl alcohol does heating in water bath for reaction under conditions of solvent, and Bi-phenolic Methan e epoxy resin, which divides 3 times, to feed intake, control reaction
Temperature is 55 DEG C, insulated and stirred 1h after feeding intake.In the reaction solution for weighing a certain amount of phosphorous acid investment again, warming-in-water is extremely
65 DEG C, under alcohol reflux state, 10% carbon disulfide ethanol solution, time for adding 3h, after completion of dropwise addition are added dropwise while stirring
Insulation reaction 2h adds a small amount of sodium hydrate solid, and the alcohol solvent in reaction solution is sloughed in vacuum distillation after ten minutes for stirring
And small-molecule substance, vacuum drying presses table 1 to get high-molecular chelating agent, the mol ratio of reaction mass at 50 DEG C of resultant product
Shown in the ratio of middle A5.
By the parts by weight of each component shown in table 3, chelating agent, modification of chitosan, polyacrylamide, meta-aluminic acid are weighed
Sodium is put into round-bottomed flask, and a small amount of water is added under room temperature and is mixed evenly, pours into mold and is dried in vacuo, and absorption is made
Agent product, number is B1, B2, B3, B4, B5 as shown in table 3.
The different embodiments of table 3 prepare parts by weight shared by each component in adsorbent
| Prepare adsorbent | Chelating agent | Modification of chitosan | Polyacrylamide | Sodium metaaluminate |
| B1 | 5 | 3 | 2 | 1 |
| B2 | 4 | 3 | 2 | 3 |
| B3 | 4 | 4 | 3 | 2 |
| B4 | 5 | 4 | 2 | 2 |
| B5 | 6 | 2 | 2 | 1 |
Embodiment 4：Adsorption effect of the adsorbent of different process index to water intermediate ion
Adsorbent B 1, B2, B3, B4, B5 are studied to Ca in water2+、Mg2+、Zn2+、Fe2+The adsorption effect of ion.Measure six parts
1L polycarboxylate water-reducer synthesis water, number 1-6 is spare, weighs 0.4g adsorbent B 1-B5 respectively, and the diminishing of number 1-5 is added
With in water, adsorbent is not added as blank group in number 6 for agent synthesis, is stood after stirring 1h under room temperature, is deposited in test water
The precipitating time completely used.The completely rear filtering of precipitating, using the Ca of Atomic Absorption Spectrometry amount filtrate2+、Mg2+、Zn2+、
Fe2+Ion concentration, each sample measurement are averaged three times, and data record is as shown in table 4.
The ion concentration of water and precipitating complete time after the different adsorbent processing of table 4
In conjunction with table 3 and table 4 it is found that changing the quality proportioning of chelating agent, chitosan, polyacrylamide, sodium metaaluminate, preparation
The performance of adsorbent have apparent difference, the deposition rate of adsorbent is not also identical, and main cause is chelating agent to adsorbent
Deposition rate have a significant effect, increase its quality proportioning, the sorbent deposition rate of preparation is accelerated, but the too fast rate of adsorption
The ion being unfavorable in water removal.Chitosan, polyacrylamide and sodium metaaluminate primarily serve Ca in absorption water2+、Mg2+、Zn2 +、Fe2+The effect of ion increases the quality proportioning of three, can accelerate adsorbent to the rate of adsorption of water intermediate ion, more favorably
In the various ions gone in water removal.It is comprehensively compared, the preparation process and adsorption effect of adsorbent B 4 are more excellent.
Embodiment 5：Ion concentration in different adsorbent amounts treated water
Ion concentration in select adsorbent B 4 to study different adsorbent amounts treated water.Different amounts of B4 is weighed to inhale
Attached dose of processing high performance water-reducer water, adsorbent amount (adsorbent mass being added in 1L water) be respectively 0.1g/L, 0.2g/L,
0.3g/L, 0.4g/L, 0.5g/L, 0.8g/L, 1.0g/L are adopted by using high performance water-reducer water is handled the step of embodiment 2-1
The Ca of water after being handled with Atomic Absorption Spectrometry amount2+、Mg2+、Zn2+、Fe2+Ion concentration, each sample measurement are averaged three times
Value, data are as depicted in figs. 1 and 2.
By Fig. 1 and Fig. 2 it is found that adsorbent amount has apparent influence, Ca in untreated water to the content of water intermediate ion2 +、Mg2+Total content 14.15mg/L, Zn2+、Fe2+Total content 1.36mg/L, with the addition of adsorbent, the Ca of water2+、Mg2+、Zn2 +、Fe2+Ion concentration rapid decrease, after adsorbent amount is greater than 0.5g/L, the decline of water ions content slows down, adsorbent amount
When 1.0g/L, Ca2+、Mg2+、Zn2+、Fe2+Ion concentration levels off to zero substantially, shows adsorbent to residual in high performance water-reducer water
Remaining Ca, Mg and Fe zinc ion has extraordinary removal effect.
Embodiment 6：Influence of adsorbent treated the water to synthesis water-reducing agent quality
Influence of adsorbent treated the water to synthesis water-reducing agent quality is studied, a certain amount of processing of adsorbent B 4 is weighed and subtracts
The synthesis water of aqua, adsorbent amount are respectively 0.1g/L, 0.3g/L, 0.5g/L, 0.8g/L, 1.0g/L, under same process
Treated water and untreated synthesis water are selected, polycarboxylate water-reducer product is respectively synthesized, according to GB/T 8077-2000
《Methods for testing uniformity of concrete admixture》Flowing degree of net paste of cement test is carried out to sintetics, while testing sintetics
Color value, each index measurement is averaged three times, and data record is as shown in table 5.
The paste flowing degree and color value of the synthesis water-reducing agent product of table 5
As shown in Table 5, the index of untreated water and treated water sintetics has apparent difference, cement paste stream
Dynamic degree phase difference is up to 45mm, and initial product color is essentially identical, but after placing 7 days under room temperature, it is untreated be hydrated at
Water-reducing agent product, color value significantly increases, and product color is obviously deepened, the color value of adsorbent treated water sintetics
It being held essentially constant, product is colorless and transparent, this illustrates that adsorbent has a great impact to the quality of high performance water-reducer product,
And with the increase of adsorbent amount, the index for synthesizing water-reducing agent product gradually improves, and after adsorbent amount is greater than 0.5g/L, produces
The variation of product index value tends towards stability, and considering cost factor selects 0.5~0.8g/L of adsorbent amount to handle high performance water-reducer
It is relatively reasonable with water.
The above content is the preferred embodiments of combination the invention to further detailed made by provided technical solution
Describe in detail bright, and it cannot be said that the invention specific implementation is confined to these above-mentioned explanations, technology affiliated for the invention
For the those of ordinary skill in field, without departing from the concept of the premise of the invention, several simple deductions can also be made
Or replacement, it all shall be regarded as belonging to the protection scope of the invention.
Claims (10)
1. a kind of adsorbent, it is characterised in that：The adsorbent includes high-molecular chelating agent, modification of chitosan, polyacrylamide
And sodium metaaluminate, the high-molecular chelating agent molecular structure are
。
2. a kind of adsorbent as described in claim 1, it is characterised in that：The adsorbent is by high-molecular chelating agent, modification
Chitosan, polyacrylamide and sodium metaaluminate mix, and mixing mass ratio is：
Chelating agent 4 ~ 6,
Modification of chitosan 2 ~ 5,
Polyacrylamide 2 ~ 3,
Sodium metaaluminate 1 ~ 2.
3. a kind of adsorbent as claimed in claim 2, it is characterised in that：The average molecular weight of the chelating agent is 1200 ~
1500g/mol。
4. a kind of adsorbent as described in claim 1, it is characterised in that：The modification of chitosan is through monoxone and hydroxide
The modified carboxymethyl chitosan powder of sodium.
5. the preparation method of adsorbent according to any one of claims 1-4, which is characterized in that include the following steps：
（1）It weighs Isosorbide-5-Nitrae-butanediamine to be dissolved in dehydrated alcohol, heating water bath is to 40-60 DEG C, under alcohol reflux state, is added
Bi-phenolic Methan e epoxy resin keeps temperature-resistant stirring 30-60min, obtains intermediate product solution A；
（2）It weighs in sodium phosphite investment solution A, is warming up to 40-60 DEG C, is stirred at reflux under state, carbon disulfide ethyl alcohol is added dropwise
Solution, insulation reaction 1-4h after completion of dropwise addition add sodium hydrate solid, and after stirring 5-30 minutes, production is sloughed in vacuum distillation
Alcohol solvent and small-molecule substance in object are dried in vacuo at 45-55 DEG C of resultant product, and secure satisfactory grades sub- chelating agent；
（3）Modification of chitosan, polyacrylamide, sodium metaaluminate and step are weighed in parts by weight（2）What is synthesized is high-molecule chelated
Agent is put into flask, and under room temperature plus water is mixed evenly, and is dried in vacuo to get product adsorbent.
6. sorbent preparation method as claimed in claim 5, it is characterised in that：The Bi-phenolic Methan e epoxy resin is averaged
Molecular weight is 514g/mol.
7. sorbent preparation method as claimed in claim 5, it is characterised in that：Step（1）In, the Bi-phenolic Methan e epoxy
Resin is with Isosorbide-5-Nitrae-butanediamine molar ratio（2-2.5）：1, hybrid reaction temperature is 50-55 DEG C.
8. sorbent preparation method as claimed in claim 5, it is characterised in that：Step（2）In, the carbon disulfide ethyl alcohol is molten
The time for adding of liquid is 2.5-3h, and drip reacting temperature is 60-70 DEG C；The sodium phosphite and Isosorbide-5-Nitrae-butanediamine molar ratio
It is（1-1.5）：1, the molar ratio of carbon disulfide and Isosorbide-5-Nitrae butanediamine is（1 -1.5）:1.
9. sorbent preparation method as claimed in claim 5, it is characterised in that：Step（3）In, modification of chitosan and Isosorbide-5-Nitrae-
The molar ratio of butanediamine is 1-2.5：1.
10. the application of adsorbent as described in claim any one of 1-4, it is characterised in that：Adsorbent is used to remove water-reducing agent
Ca in synthetic water2+、Mg2+、Fe2+、Zn2+When ion, the dosage of adsorbent is not less than 0.5g/L.
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| US8518269B2 (en) * | 2011-03-30 | 2013-08-27 | Crystal Lagoons (Curacao) B.V. | Method and system for treating water used for industrial purposes |
| CN104437395A (en) * | 2014-11-03 | 2015-03-25 | 中国科学院过程工程研究所 | Acid-resistant magnetic chitosan microspheres as well as preparation method and application thereof |
| CN104788606A (en) * | 2015-04-09 | 2015-07-22 | 太原理工大学 | Magnetic water-absorbent resin as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8518269B2 (en) * | 2011-03-30 | 2013-08-27 | Crystal Lagoons (Curacao) B.V. | Method and system for treating water used for industrial purposes |
| CN104437395A (en) * | 2014-11-03 | 2015-03-25 | 中国科学院过程工程研究所 | Acid-resistant magnetic chitosan microspheres as well as preparation method and application thereof |
| CN104788606A (en) * | 2015-04-09 | 2015-07-22 | 太原理工大学 | Magnetic water-absorbent resin as well as preparation method and application thereof |
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