CN106916260A - A kind of preparation method of hud typed porous high water absorption microballoon - Google Patents
A kind of preparation method of hud typed porous high water absorption microballoon Download PDFInfo
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a kind of preparation method of hud typed porous high water absorption microballoon, comprise the following steps：（1）Acrylic or methacrylic acid is added in deionized water, is neutralized with sodium hydroxide solution under normal temperature；It is subsequently added non-ionic monomer；（2）Sequentially add sodium alginate, crosslinking agent, initiator and pore-foaming agent；（3）Dimethicone is taken, calcium chloride solution is subsequently added；After profit is mutually layered, heating oil phase instills reaction solution and is reacted to 60~80 DEG C.（4）After reaction terminates, washing, desciccate.The present invention uses various pore-foaming agent compound uses, granulation process is set to be completed before polymerisation by the solidification of sodium alginate, and microballoon forms the Calcium alginate film with certain elasticity and hardness after granulation, after into oil phase without by stirring-granulating and will not the blocking calcium alginate films of adhesion microballoon can also be made to absorb water after still keep certain intensity, expand range of application.
Description
Technical field
The present invention relates to high hydroscopic resin technology, more specifically to the preparation method of acrylic acid series high water absorption microballoon.
Background technology
High hydroscopic resin（Super Absorbent Resin, abbreviation SAR）It is to start to grow up the sixties in 20th century
Novel high polymer material, with rapid development of economy and the raising of people's living standard and the enhancing of environmental consciousness, SAR's
Range of application constantly expands, and the market demand increasingly increases, and research and development is also increasingly active.Wherein, polyacrylate is high
Water-absorbing resin is to study and produce most class synthesizing super absorbent resins at present, and this kind of product water absorption rate is higher, up to thousand times
More than.
High hydroscopic resin is produced with water solution polymerization process mostly in current industrial production, what Later development got up mainly has anti-
Phase suspension polymerization.Because inverse suspension polymerization has the advantages that to be easy to heat transfer, uniform particle sizes etc., more and more passes are therefore suffered from
Note.Patent document such as Publication No. CN 1834122A has invented a kind of use inverse suspension polymerization and has synthesized polyacrylic acid
（Salt）High hydroscopic resin.But inverse suspension polymerization has the complex process of recycling design, dispersant, this causes its development to be subject to
Certain limitation.
The high hydroscopic resin of current production can reach liquid absorbency rate high, so sight is turned on imbibition by researchers
In the problem of speed.How quick imbibition is realized, how to make resin that gel strength higher is still kept after imbibition is people
Of interest.In this context, porous water-absorbing resin arises at the historic moment, and good pore structure can provide bigger specific surface
Product, plays the role of positive to liquid absorbency rate and rate of liquid aspiration；Irrational pore structure can then play opposite effect, especially
Resin collapse of pore structure after imbibition, gel strength is substantially reduced, and hinders the further infiltration of moisture.In sum, hole knot is prepared
Structure is reasonable, uniform high water absorption microballoon is still a research topic being significant.
The content of the invention
It is contemplated that the rational porous resin of pore structure is built, to improve the rate of liquid aspiration of resin.The present invention passes through
One layer of Calcium alginate film is coated in resin surface, gel strength is low after expecting to solve the problems, such as resin water suction.
To achieve the above object, the present invention adopts the following technical scheme that its step includes：
A kind of preparation method of hud typed porous high water absorption microballoon, comprises the following steps：
（1）Anionic monomer acrylic acid or methacrylic acid are added in deionized water, with sodium hydroxide solution under normal temperature
With it is 55~75% to control degree of neutralization；It is subsequently added nonionic monomer acrylamide, propenyl APEO, pentaerythrite alkene
Propyl ether, it is anionic monomer to control monomer mass：Non-ionic monomer=2：1~4：1；
（2）Sodium alginate, crosslinking agent, initiator and pore-foaming agent are sequentially added, relative to the quality of monomer, its consumption is respectively：1
~3%, 0.25~1%, 0.01~0.5%, 5~20%；
（3）The dimethicone that viscosity is 50~100mPas is taken, the calcium chloride that mass fraction is 5~15% is subsequently added molten
Liquid；After profit is mutually layered, heating oil phase instills reaction solution and is reacted to 60~80 DEG C；Reaction medium is divided into water layer and oil
Layer, water layer is calcium chloride solution, and oil reservoir is dimethicone, and water layer solution pillar height is more than 5cm.Reaction drop is introduced into water layer and consolidates
Chemical conversion ball, continues to react subsequently into oil reservoir.Size droplet diameter is controlled to 0.5~3mm, and final microballoon shell coats a tunic thickness and is
50~300 μm of Calcium alginate films.
（4）After reaction terminates, washing, desciccate obtain the porous high water absorption microballoon of pearl.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, the initiator is azo
The compound of initiator and persulfuric acid salt initiator, wherein azo are the isobutyl imidazole hydrochloride of azo two, the isobutyl of azo two
Base amidine hydrochloride or azo dicyclohexyl formonitrile HCN.Persulfate is potassium peroxydisulfate or ammonium persulfate, and mass ratio is controlled to azo
Class：Persulfuric acid salt=3：1~5：1.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, the pore-foaming agent is mixed for ternary
Compound, a urmaterie be sodium acid carbonate, saleratus in one or two；Binary substance is urea；Ternary materials are ethanol
With one or two the compound in acetone；The mass ratio of ternary materials is controlled to 1：3：2 or 1：3：1 or 1：2：2 or 1：2：
3.One should with carboxyl reaction or itself can decompose generation gas, one need to water at 100 DEG C or so generated reactive gas,
One should be easy to volatilization and not with monomer reaction.
As preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, step（4）Described dries temperature
It is 80~100 DEG C to spend, and drying time is 6~8h.
As preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, while pore-foaming agent is added,
Also add coloring agent, aromatic, fertilizer or magnetisable material.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, the crosslinking agent is polynary alkene
One or more in propyl group or diolefin crosslinking agent.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, the polynary pi-allyl is alkene
Propylated starches, allylation cellulose or tetraallyl epoxide ethane；The diolefin crosslinking agent is N, N '-di-2-ethylhexylphosphine oxide
Acrylamide.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, being provided with reaction vessel to go up
The filter vat of lower movement, residence time of the microballoon in water layer and oil reservoir that absorb water is controlled by controlling the position of filter vat.Instead
After should terminating, lift filter vat and collect microballoon, wherein, filter vat is made up of the screen cloth of 100 mesh.
Used as preferred, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, the reaction solution passes through pore
Device is added dropwise over, and size droplet diameter is 0.5~3mm.
Compared with prior art, the present invention has the advantages that：
The present invention uses various pore-foaming agent compound uses, and three kinds of pore mechanism of pore-foaming agent are different, compared to single pore-foaming agent
Effect, the present invention obtained by pore structure size reasonable, be evenly distributed, ensure that the quantity of pore structure.The present invention passes through
The solidification of sodium alginate makes granulation process be completed before polymerisation, and after granulation microballoon formed have it is certain it is elastic with it is hard
The Calcium alginate film of degree, into oil phase after without by stirring-granulating and will not adhesion it is blocking, therefore need not using suspend
Stabilizer.Calcium alginate film can also make microballoon still keep certain intensity after absorbing water, and expand range of application.In reaction unit
Filter vat is installed, reaction can directly lift filter vat and collect product after terminating, easy to operate and safe.
Brief description of the drawings
Fig. 1 is the schematic diagram of pore dropper.
1 is charge door, and 2 is nitrogen inlet, and 3 is capillary or the tubule with thin mouth nozzle, and 4 is filter vat, and 5 is removable
Dynamic adjuster.
Fig. 2 is that the metallography microscope of water suction microballoon and SEM scheme.
Fig. 3 is microballoon rate of water absorption figure.
Fig. 4 is the microballoon aspect graph for whetheing there is cured layer.
Specific embodiment
Embodiment 1：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 26g+ deionized waters 60.67g）It is 65% to be neutralized to degree of neutralization.It is subsequently adding 24.02g propylene
Acid amides.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：1g, tetraallyl epoxide ethane：0.48g, azo
Two isobutyl imidazole hydrochlorides：0.2g, potassium peroxydisulfate：0.025g, sodium acid carbonate：1.6g, urea：4.8g, ethanol：3.2g.Mixing
It is uniform standby.
（3）The dimethicone that 300g viscosity is 50mPas is taken, the calcium chloride solution that 100g mass fractions are 5% is delayed
Slowly pour into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lifted
Lauter tub collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 85 DEG C of constant temperature blast drying oven, final to obtain
To hud typed porous water-absorbing microballoon.As shown in figure 1,1 is charge door, 2 is nitrogen inlet, and 3 are for the schematic diagram of pore dropper
Capillary or the tubule with thin mouth nozzle, 4 is filter vat, and 5 is removable adjuster.Gained water suction microballoon core shell structure with
Pore structure is shown in Fig. 2, and metallurgical microscopic and the SEM of microballoon a quarter section scheme, and shell is thick to be about the 1/10 of core thickness.Before and after pore,
Microballoon rate of water absorption compares sees Fig. 3.The microballoon form for whetheing there is cured layer is shown in Fig. 4.
Embodiment 2：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 28g+ deionized waters 65.33g）It is 70% to be neutralized to degree of neutralization.It is subsequently adding 18.02g propylene
Alcohol APEO.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：1.5g, tetraallyl epoxide ethane：0.24g, N,
N '-methylene-bisacrylamide：0.24g, the isobutyl imidazole hydrochloride of azo two：0.2g, ammonium persulfate：0.025g, bicarbonate
Potassium：1.6g, urea：4.8g, acetone：3.2g.It is well mixed standby.
（3）The dimethicone that 300g viscosity is 50mPas is taken, the calcium chloride solution that 100g mass fractions are 7% is delayed
Slowly pour into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lifted
Lauter tub collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 85 DEG C of constant temperature blast drying oven, final to obtain
To hud typed porous water-absorbing microballoon.
Embodiment 3：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 30g+ deionized waters 100g）It is 75% to be neutralized to degree of neutralization.It is subsequently adding 18.02g seasons penta 4
Alcohol allyl ether.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：2g, allylation starch：0.48g, azo two is different
Butyl Amidine HCl salt：0.2g, potassium peroxydisulfate：0.05g, saleratus：1.6g, urea：4.8g, acetone：1.6g, ethanol：1.6g.
It is well mixed standby.
（3）The dimethicone that 300g viscosity is 50mPas is taken, the calcium chloride solution that 100g mass fractions are 9% is delayed
Slowly pour into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lifted
Lauter tub collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 85 DEG C of constant temperature blast drying oven, final to obtain
To hud typed porous water-absorbing microballoon.
Embodiment 4：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 28g+ deionized waters 65.33g）It is 70% to be neutralized to degree of neutralization.It is subsequently adding 18.02g propylene
Acid amides, 6g pentaerythrite allyl ethers.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：2.25g, allylation starch：0.24g, N,
N '-methylene-bisacrylamide：0.24g, azo diisobutyl amidine hydrochloride：0.2g, ammonium persulfate：0.05g, sodium acid carbonate：
1.6g, urea：4.8g, ethanol：1.6g.It is well mixed standby.
（3）The dimethicone that 300g viscosity is 100mPas is taken, by the calcium chloride solution that 100g mass fractions are 11%
It is poured slowly into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lift
Filter vat collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 85 DEG C of constant temperature blast drying oven, finally
Obtain hud typed porous water-absorbing microballoon.
Embodiment 5：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 28g+ deionized waters 65.33g）It is 70% to be neutralized to degree of neutralization.It is subsequently adding 12.01g propylene
Acid amides, 12.01g propenyl APEOs.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：2.5g, allylation cellulose：0.48g, azo
Diisopropyl imidazoline：0.2g, potassium peroxydisulfate：0.067g, saleratus：1.6g, urea：4.8g, ethanol：0.8g, acetone：
0.8g.It is well mixed standby.
（3）The dimethicone that 200g viscosity is 100mPas is taken, by the calcium chloride solution that 100g mass fractions are 13%
It is poured slowly into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lift
Filter vat collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 100 DEG C of constant temperature blast drying oven, most
Hud typed porous water-absorbing microballoon is obtained eventually.
Embodiment 6：
（1）72.06g acrylic acid is added in 38.88g deionized waters, is well mixed, with mass fraction be 30% under normal temperature
Sodium hydroxide solution（NaOH 28g+ deionized waters 65.33g）It is 70% to be neutralized to degree of neutralization.It is subsequently adding 8.01g acryloyls
Amine, 8.01g propenyl APEOs, 8.01g pentaerythrite allyl ethers.
（2）Liquid to be neutralized is cooled to room temperature, sequentially adds sodium alginate：2.5g, allylation cellulose：024g, N,
N '-methylene-bisacrylamide：0.24g, azo dicyclohexyl formonitrile HCN：0.2g, ammonium persulfate：0.067g, sodium acid carbonate：
0.8g, saleratus：0.8g, urea：4.8g, ethanol：1.6g, acetone：1.6g.It is well mixed standby.
（3）The dimethicone that 200g viscosity is 100mPas is taken, by the calcium chloride solution that 100g mass fractions are 15%
It is poured slowly into dimethicone.After profit layering, heating oil phase is added dropwise over reaction solution to 70 DEG C.After reaction terminates, lift
Filter vat collects product, is washed with ethyl acetate three times, is then placed into drying 8h in 100 DEG C of constant temperature blast drying oven, most
Hud typed porous water-absorbing microballoon is obtained eventually.
Claims (10)
1. a kind of preparation method of hud typed porous high water absorption microballoon, it is characterised in that comprise the following steps：
（1）Anionic monomer acrylic acid or methacrylic acid are added in deionized water, with sodium hydroxide solution under normal temperature
With it is 55~75% to control degree of neutralization；It is subsequently added nonionic monomer acrylamide, propenyl APEO or pentaerythrite
Allyl ether, it is anionic monomer to control monomer mass：Non-ionic monomer=2：1~4：1；
（2）Sodium alginate, crosslinking agent, initiator and pore-foaming agent are sequentially added, relative to the quality of monomer, its consumption is respectively：1
~3%, 0.25~1%, 0.01~0.5%, 5~20%；
（3）The dimethicone that viscosity is 50~100mPas is taken, the calcium chloride that mass fraction is 5~15% is subsequently added molten
Liquid；After profit is mutually layered, heating oil phase instills reaction solution and is reacted to 60~80 DEG C；
（4）After reaction terminates, washing, desciccate obtain the porous high water absorption microballoon of pearl.
2. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that the initiator is
The compound of azo-initiator and persulfuric acid salt initiator, wherein azo are the isobutyl imidazole hydrochloride of azo two, azo
Diisobutyl amidine hydrochloride or azo dicyclohexyl formonitrile HCN, persulfate are potassium peroxydisulfate or ammonium persulfate, mass ratio control
It is azo：Persulfuric acid salt=3：1~5：1.
3. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that pore-foaming agent is ternary
Mixture, a urmaterie be sodium acid carbonate, saleratus in one or two；Binary substance is urea；Ternary materials are second
One or two compound in alcohol and acetone；The mass ratio of ternary materials is controlled to 1：3：2 or 1：3：1 or 1：2：2 or 1：
2：3.
4. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that step（4）It is described
Drying temperature be 80~100 DEG C, drying time be 6~8h.
5. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that in addition pore-foaming agent
While, also add coloring agent, aromatic, fertilizer or magnetisable material.
6. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that the crosslinking agent is
One or more in polynary pi-allyl or diolefin crosslinking agent.
7. the preparation method of hud typed porous high water absorption microballoon according to claim 6, it is characterised in that the polynary allyl
Base is allylation starch, allylation cellulose or tetraallyl epoxide ethane；The diolefin crosslinking agent is N, N '-Asia
Bisacrylamide.
8. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that set in reaction vessel
Have a filter vat moving up and down, after reaction terminates, microballoon collected by filter vat, filter vat bottom surface by 100 mesh screen cloth system
Into.
9. the preparation method of hud typed porous high water absorption microballoon according to claim 1, it is characterised in that the reaction solution leads to
Cross pore dropper to be added dropwise over, size droplet diameter is 0.5~3mm.
10. a kind of hud typed porous high water absorption microballoon, it is characterised in that by the method system described in any one of claim 1~9
It is standby to obtain.
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| CN107935189A (en) * | 2017-12-14 | 2018-04-20 | 陈英 | A kind of technique using algae microballoon processing sanitary sewage |
| CN111718438A (en) * | 2019-03-20 | 2020-09-29 | 华东理工大学 | Preparation method of porous sodium polyacrylate super absorbent resin |
| CN114790264A (en) * | 2022-05-12 | 2022-07-26 | 兰州理工大学 | Spherical gel particles and preparation method and application thereof |
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| CN114790264A (en) * | 2022-05-12 | 2022-07-26 | 兰州理工大学 | Spherical gel particles and preparation method and application thereof |
| CN114790264B (en) * | 2022-05-12 | 2024-04-05 | 兰州理工大学 | Spherical gel particles and preparation method and application thereof |
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| CN114907513B (en) * | 2022-06-28 | 2024-04-02 | 广东石油化工学院 | Preparation method of spherical high-performance water-absorbing microsphere and product thereof |
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