CN105524232A - Preparation method of humidity-adjusting adsorption composite porous chelating resin - Google Patents
Preparation method of humidity-adjusting adsorption composite porous chelating resin Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/02—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of acids, salts or anhydrides
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/20—Organic adsorbents
- B01D2253/202—Polymeric adsorbents
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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
- B01J2220/44—Materials comprising a mixture of organic materials
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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
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a preparation method of humidity-adjusting adsorption composite porous chelating resin. The preparation method includes the following steps: (1) preparation of a porous resin matrix; (2) washing and drying; (3) surface grafting; (4) complexation reaction; and (5) polymerization reaction. The invention relates to the preparation method of the humidity-adjusting adsorption composite porous chelating resin; the preparation method is simple to operate and easy to realize; through scientific formula design and reasonable preparation process design, firstly, composite porous resin microspheres are prepared, then the surface of the composite porous resin microspheres is grafted and polymerized with a polymer having heavy metal ion chelation, and thus the composite resin integrating functions of humidity adjustment, gas absorption and metal ion adsorption is prepared; the composite resin has excellent humidity-adjusting performance, low-concentration formaldehyde adsorption performance and heavy metal ion chelating adsorption performance, can highly purify air, is functional resin with excellent comprehensive performance and for green buildings, and has the advantages of excellent comprehensive performance and broad market prospects.
Description
Technical field
The present invention relates to functional resin field, particularly relate to the preparation method that compound porous resin is adsorbed in a kind of damping.
Background technology
Along with the enhancing of people's energy-conserving and environment-protective consciousness, the material of construction possessing energy-conserving and environment-protective and green ecological function more and more receives publicity.At present, serious due to air environmental pollution, the demand of people to the humidity conditioning function of material of construction and adsorption filtration function significantly improves.Humidity-controlling functional material turns to the research of porous resin, organic/inorganic compound, biological material gradually from the research of traditional inorganic salts, silica gel, inorganic mineral class, and it mainly utilizes in the vesicular structure of inorganic mineral and organic macromolecule height moisture content and biomass a large amount of moisture absorptions contained to guide groups.This hygroscopic material to gas pollutant as formaldehyde etc. has certain adsorptive power, but poor for the adsorptive power of solid particulate as heavy metal, and it is not obvious to the adsorption effect of low concentration formaldehyde, can not meet the need of market.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method with the compound porous resin of damping and adsorption filtration function, can solve the weak point that existing capability material exists in low concentration formaldehyde and the absorption of heavy metal particles pollutent.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of damping to adsorb the preparation method of compound porous resin, comprise the steps:
(1) prepare porous resin matrix: get that weight part is the acrylamide of 40 ~ 50 parts, the sodium polyacrylate of 10 ~ 15 parts, the Xylo-Mucine of 10 ~ 15 parts, the letex polymerization promotor of 3 ~ 5 parts, the dispersion agent of 1 ~ 3 part and 15 ~ 20 parts filler be dissolved in appropriate amount of deionized water, after being uniformly mixed, add first cross-linked evocating agent of 3 ~ 5 parts, under atmosphere of inert gases, heated and stirred reaction is to occurring gel state, then add second cross-linked evocating agent of 8 ~ 12 parts, continue stirring reaction certain hour;
(2) washing is dry: by the reaction product organic solvent washing in step (1), after drying, grind to form microballoon;
(3) surface grafting: add in the microballoon obtained in step (2) that weight part is 0.1 ~ 0.3 part 2, the catalyzer of 2 '-bipyridine, the glycidyl methacrylate of 5 ~ 15 parts, the tetrahydrofuran (THF) of 15 ~ 20 parts and 0.05 ~ 0.15 part, mixing and stirring, then liquid nitrogen freezing vacuumizes, and passes into N after thawing
2gas circulates 3 times, then isothermal reaction;
(4) complex reaction: the complexometric reagent adding 50 ~ 100 parts in the Surface grafting reaction thing in step (3), stirs and makes it to carry out complex reaction, then wash, vacuum-drying;
(5) polyreaction: getting dried complexing product in step (4), to insert weight part be in the iminodiacetic acid (salt) acid solution of 20 ~ 30 parts, add the formaldehyde of 10 ~ 20 parts again, regulate the pH value of mixing solutions to alkalescence, then heated and stirred makes it reaction, and reaction terminates the pH value of rear adjustment mixing solutions to acid, still aging, finally filter, washing, vacuum-drying, obtains described damping and adsorbs compound porous resin.
In a preferred embodiment of the present invention, in described step (1), described letex polymerization promotor is Sodium Persulfate or Potassium Persulphate; Described dispersion agent is N, N '-methylene-bisacrylamide; Described filler is the sepiolite of mass ratio 2 ~ 3:1 and the mixture of tourmaline powder; Described first linking agent is aluminum chloride; Described second linking agent is sodium bicarbonate.
In a preferred embodiment of the present invention, in described step (1), described Heating temperature is 75 ~ 80 DEG C, and the described stirring reaction time is 5 ~ 8h.
In a preferred embodiment of the present invention, in described step (2), described drying means is under 0.1 ~ 0.3MPa vacuum tightness, first with 60 ~ 70 DEG C of dry 30min, then at 120 ~ 130 DEG C dry 60 ~ 90min; Median size after described grinding is 10 ~ 50 μm.
In a preferred embodiment of the present invention, in described step (3), described catalyzer is cuprous bromide; The condition of described isothermal reaction is temperature 50 ~ 80 DEG C, time 1 ~ 3h.
In a preferred embodiment of the present invention, in described step (4), described complexometric reagent is the mixing solutions that methyl alcohol, ethylenediamine tetraacetic acid (EDTA) and water mix with the mass ratio of 1:2 ~ 3:3 ~ 5.
In a preferred embodiment of the present invention, in described step (5), described alkaline ph values is 9.5 ~ 10; Described acid ph value is 3.5 ~ 4; Described Heating temperature is 90 ~ 100 DEG C, and the reaction times is 8 ~ 10h.
In a preferred embodiment of the present invention, in described step (4) and (5), described vacuum tightness is 0.1 ~ 0.3MPa, and drying temperature is 55 ~ 60 DEG C.
The invention has the beneficial effects as follows: the preparation method of compound porous resin is adsorbed in a kind of damping of the present invention, easy and simple to handle, easy realization, its formulating of recipe by science and rational preparation technology design, first prepare composite porous resin microballoon, there is at its surface grafting polymerization the polymkeric substance of heavy metal ion sequestering action again, thus prepare there is damping, gas absorption and adsorption of metal ions function are in the compound resin of one, this compound resin has excellent humidity, low concentration formaldehyde absorption property and heavy metal ion chelating absorption property, high purification can be carried out to air, it is a kind of green building functional resin of excellent combination property, excellent combination property, wide market.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
A preparation method for compound porous resin is adsorbed in damping, comprises the steps:
(1) porous resin matrix is prepared: getting weight part is the acrylamide of 40 parts, the sodium polyacrylate of 10 parts, the Xylo-Mucine of 10 parts, the Sodium Persulfate of 3 parts or Potassium Persulphate, the N of 1 part, the filler of N '-methylene-bisacrylamide and 15 parts is dissolved in appropriate amount of deionized water, after being uniformly mixed, add the aluminum chloride of 3 parts, 75 DEG C are heated under atmosphere of inert gases, stirring reaction, to there is gel state, then adds the sodium bicarbonate of 8 parts, and constant temperature continues stirring reaction 5h; Described filler is the sepiolite of mass ratio 2:1 and the mixture of tourmaline powder;
(2) washing is dry: washed by the organic solvent (ethanol) of the reaction product in step (1), under 0.1 ~ 0.3MPa vacuum tightness, first with 60 DEG C of dry 30min, then at 120 DEG C dry 60 ~ 90min, after drying, median size is become to be the microballoon of 10 ~ 50 μm with ball mill grinding;
(3) surface grafting: add in the microballoon obtained in step (2) that weight part is 0.1 part 2, the cuprous bromide of 2 '-bipyridine, the glycidyl methacrylate of 5 parts, the tetrahydrofuran (THF) of 15 parts and 0.05 part, mixing and stirring, then liquid nitrogen freezing vacuumizes, and passes into N after thawing
2gas circulates 3 times, then at 50 DEG C isothermal reaction 3h;
(4) complex reaction: the complexometric reagent adding 50 parts in the Surface grafting reaction thing in step (3), stirs and makes it to carry out complex reaction, then wash, the lower 55 DEG C of dryings of 0.1 ~ 0.3MPa vacuum tightness; Described complexometric reagent is the mixing solutions that methyl alcohol, ethylenediamine tetraacetic acid (EDTA) and water mix with the mass ratio of 1:2:3;
(5) polyreaction: getting dried complexing product in step (4), to insert weight part be in the iminodiacetic acid (salt) acid solution of 20 parts, add the formaldehyde of 10 parts again, the pH value regulating mixing solutions is 9.5, then be heated to 90 DEG C of stirrings make it to react 8h, the pH value that reaction terminates rear adjustment mixing solutions is 3.5, still aging 1h, finally filter, washing, vacuum-drying, obtains described damping and adsorbs compound porous resin.
Embodiment 2
A preparation method for compound porous resin is adsorbed in damping, comprises the steps:
(1) porous resin matrix is prepared: getting weight part is the acrylamide of 50 parts, the sodium polyacrylate of 15 parts, the Xylo-Mucine of 15 parts, the Sodium Persulfate of 5 parts or Potassium Persulphate, the N of 3 parts, the filler of N '-methylene-bisacrylamide and 20 parts is dissolved in appropriate amount of deionized water, after being uniformly mixed, add the aluminum chloride of 5 parts, 80 DEG C are heated under atmosphere of inert gases, stirring reaction, to there is gel state, then adds the sodium bicarbonate of 12 parts, and constant temperature continues stirring reaction 8h; Described filler is the sepiolite of mass ratio 3:1 and the mixture of tourmaline powder;
(2) washing is dry: washed by the organic solvent (ethanol) of the reaction product in step (1), under 0.1 ~ 0.3MPa vacuum tightness, first with 70 DEG C of dry 30min, then at 130 DEG C dry 90min, after drying, median size is become to be the microballoon of 10 ~ 50 μm with ball mill grinding;
(3) surface grafting: add in the microballoon obtained in step (2) that weight part is 0.3 part 2, the cuprous bromide of 2 '-bipyridine, the glycidyl methacrylate of 15 parts, the tetrahydrofuran (THF) of 20 parts and 0.15 part, mixing and stirring, then liquid nitrogen freezing vacuumizes, and passes into N after thawing
2gas circulates 3 times, then at 80 DEG C isothermal reaction 3h;
(4) complex reaction: the complexometric reagent adding 100 parts in the Surface grafting reaction thing in step (3), stirs and makes it to carry out complex reaction, then wash, the lower 60 DEG C of dryings of 0.3MPa vacuum tightness; Described complexometric reagent is the mixing solutions that methyl alcohol, ethylenediamine tetraacetic acid (EDTA) and water mix with the mass ratio of 1:3:5;
(5) polyreaction: getting dried complexing product in step (4), to insert weight part be in the iminodiacetic acid (salt) acid solution of 30 parts, add the formaldehyde of 20 parts again, the pH value regulating mixing solutions is 10, then be heated to 100 DEG C of stirrings make it to react 10h, the pH value that reaction terminates rear adjustment mixing solutions is 4, still aging 1h, finally filter, washing, vacuum-drying, obtains described damping and adsorbs compound porous resin.
The compound porous resin of aforesaid method produces Al (OH) by aluminum chloride and sodium bicarbonate
3as linking agent, crosslinking polymerization produces compound resin, forming pore size distribution by pyrolytic decomposition release water vapour in compound resin inside is again the vesicular structure of 20 ~ 50nm, this composite porous resin has good humidity and formaldehyde adsorption property, and it PARA FORMALDEHYDE PRILLS(91,95) effectively can adsorb under low concentration of formaldehyde; In addition, this composite porous resin also defines grafting chelating multipolymer by surface grafting polymerization reaction, and this graft copolymer has excellent chelating adsorption to the heavy metal ion in air, thus purifies air further.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (8)
1. a preparation method for compound porous resin is adsorbed in damping, it is characterized in that, comprises the steps:
(1) prepare porous resin matrix: get that weight part is the acrylamide of 40 ~ 50 parts, the sodium polyacrylate of 10 ~ 15 parts, the Xylo-Mucine of 10 ~ 15 parts, the letex polymerization promotor of 3 ~ 5 parts, the dispersion agent of 1 ~ 3 part and 15 ~ 20 parts filler be dissolved in appropriate amount of deionized water, after being uniformly mixed, add first cross-linked evocating agent of 3 ~ 5 parts, under atmosphere of inert gases, heated and stirred reaction is to occurring gel state, then add second cross-linked evocating agent of 8 ~ 12 parts, continue stirring reaction certain hour;
(2) washing is dry: by the reaction product organic solvent washing in step (1), after drying, grind to form microballoon;
(3) surface grafting: add in the microballoon obtained in step (2) that weight part is 0.1 ~ 0.3 part 2, the catalyzer of 2 '-bipyridine, the glycidyl methacrylate of 5 ~ 15 parts, the tetrahydrofuran (THF) of 15 ~ 20 parts and 0.05 ~ 0.15 part, mixing and stirring, then liquid nitrogen freezing vacuumizes, and passes into N after thawing
2gas circulates 3 times, then isothermal reaction;
(4) complex reaction: the complexometric reagent adding 50 ~ 100 parts in the Surface grafting reaction thing in step (3), stirs and makes it to carry out complex reaction, then wash, vacuum-drying;
(5) polyreaction: getting dried complexing product in step (4), to insert weight part be in the iminodiacetic acid (salt) acid solution of 20 ~ 30 parts, add the formaldehyde of 10 ~ 20 parts again, regulate the pH value of mixing solutions to alkalescence, then heated and stirred makes it reaction, and reaction terminates the pH value of rear adjustment mixing solutions to acid, still aging, finally filter, washing, vacuum-drying, obtains described damping and adsorbs compound porous resin.
2. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (1), described letex polymerization promotor is Sodium Persulfate or Potassium Persulphate; Described dispersion agent is N, N '-methylene-bisacrylamide; Described filler is the sepiolite of mass ratio 2 ~ 3:1 and the mixture of tourmaline powder; Described first linking agent is aluminum chloride; Described second linking agent is sodium bicarbonate.
3. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (1), described Heating temperature is 75 ~ 80 DEG C, and the described stirring reaction time is 5 ~ 8h.
4. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (2), described drying means is under 0.1 ~ 0.3MPa vacuum tightness, first with 60 ~ 70 DEG C of dry 30min, then at 120 ~ 130 DEG C dry 60 ~ 90min; Median size after described grinding is 10 ~ 50 μm.
5. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (3), described catalyzer is cuprous bromide; The condition of described isothermal reaction is temperature 50 ~ 80 DEG C, time 1 ~ 3h.
6. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (4), described complexometric reagent is the mixing solutions that methyl alcohol, ethylenediamine tetraacetic acid (EDTA) and water mix with the mass ratio of 1:2 ~ 3:3 ~ 5.
7. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (5), described alkaline ph values is 9.5 ~ 10; Described acid ph value is 3.5 ~ 4; Described Heating temperature is 90 ~ 100 DEG C, and the reaction times is 8 ~ 10h.
8. the preparation method of compound porous resin is adsorbed in damping according to claim 1, it is characterized in that, in described step (4) and (5), described vacuum tightness is 0.1 ~ 0.3MPa, and drying temperature is 55 ~ 60 DEG C.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105968258A (en) * | 2016-05-27 | 2016-09-28 | 济南科慧页岩化工技术有限公司 | Clean and environmentally friendly composite polymer for fracturing fluid and preparing method thereof |
CN109232012A (en) * | 2018-09-11 | 2019-01-18 | 淮阴工学院 | Recessed soil or bentonite base plant fiber composite humidity adjusting material and its preparation method and application |
CN110835421A (en) * | 2019-12-03 | 2020-02-25 | 中北大学 | Flavonoid glycoside adsorption resin and preparation method thereof |
CN111085180A (en) * | 2019-12-12 | 2020-05-01 | 贵州师范学院 | Preparation of tannic acid based chelating adsorption resin and application of tannic acid based chelating adsorption resin in Cr (VI) adsorption |
-
2015
- 2015-12-18 CN CN201510949692.9A patent/CN105524232A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105968258A (en) * | 2016-05-27 | 2016-09-28 | 济南科慧页岩化工技术有限公司 | Clean and environmentally friendly composite polymer for fracturing fluid and preparing method thereof |
CN109232012A (en) * | 2018-09-11 | 2019-01-18 | 淮阴工学院 | Recessed soil or bentonite base plant fiber composite humidity adjusting material and its preparation method and application |
CN109232012B (en) * | 2018-09-11 | 2021-04-23 | 淮阴工学院 | Attapulgite or bentonite-based plant fiber composite humidity control material |
CN110835421A (en) * | 2019-12-03 | 2020-02-25 | 中北大学 | Flavonoid glycoside adsorption resin and preparation method thereof |
CN110835421B (en) * | 2019-12-03 | 2022-03-08 | 中北大学 | Flavonoid glycoside adsorption resin and preparation method thereof |
CN111085180A (en) * | 2019-12-12 | 2020-05-01 | 贵州师范学院 | Preparation of tannic acid based chelating adsorption resin and application of tannic acid based chelating adsorption resin in Cr (VI) adsorption |
CN111085180B (en) * | 2019-12-12 | 2022-07-05 | 贵州师范学院 | Preparation of tannic acid based chelating adsorption resin and application of tannic acid based chelating adsorption resin in Cr (VI) adsorption |
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