CN106916260B - 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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- 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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Abstract
The invention discloses a kind of preparation methods of hud typed porous high water absorption microballoon, comprising the following steps: (1) is add to deionized water acrylic or methacrylic acid, is neutralized under room temperature with sodium hydroxide solution；Non-ionic monomer is then added；(2) sodium alginate, crosslinking agent, initiator and pore-foaming agent are sequentially added；(3) dimethicone is taken, calcium chloride solution is then added；After grease is mutually layered, oil is heated mutually to 60~80 DEG C, is instilled reaction solution and is reacted.(4) after reaction, washing, desciccate.The present invention is used in combination using a variety of pore-foaming agents, granulation process is completed before polymerization reaction by the solidification of sodium alginate, and microballoon forms the Calcium alginate film with certain elasticity and hardness after being granulated, after into oily phase without by stirring-granulating and will not the blocking calcium alginate film of adhesion microballoon can also be made to absorb water after still keep certain intensity, expand application range.
Description
Technical field
The present invention relates to high hydroscopic resin technologies, more specifically to the preparation method of acrylic acid series high water absorption microballoon.
Background technique
High hydroscopic resin (Super Absorbent Resin, abbreviation SAR) is to start the 1960s to grow up
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
Application range constantly expands, and the market demand increasingly increases, and research and development also becomes more and more active.Wherein, polyacrylate is high
Water-absorbing resin is a kind of synthesizing super absorbent resin of current research and production at most, 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 industrial production at present, what Later development got up mainly has anti-
Phase suspension polymerization.Since inverse suspension polymerization has the advantages that be easy to heat transfer, uniform particle sizes etc., by more and more passes
Note.A kind of polyacrylic acid is synthesized using inverse suspension polymerization as the patent document of Publication No. CN 1834122A has been invented
(salt) high hydroscopic resin.However inverse suspension polymerization is there are the complex process of recycling design, dispersing agent, this cause its development by
Certain limitation.
The high hydroscopic resin currently produced can reach high liquid absorbency rate, so sight is turned on imbibition by researchers
On the problem of rate.How quick imbibition is realized, so that resin is still kept higher gel strength after imbibition is people
Of interest.In this context, porous water-absorbing resin comes into being, and good pore structure can provide bigger specific surface
Product plays the role of liquid absorbency rate and rate of liquid aspiration positive；Unreasonable pore structure can then play opposite effect, especially
Resin collapse of pore structure after imbibition, gel strength substantially reduce, and hinder the further infiltration of moisture.In conclusion preparation hole knot
Structure is reasonable, uniform high water absorption microballoon is still the research topic being of great significance.
Summary of the invention
The present invention is directed to construct the reasonable porous resin of pore structure, 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, it is expected that gel strength is low after solving the problems, such as resin water suction.
To achieve the above object, the present invention adopts the following technical scheme that, step includes:
A kind of preparation method of hud typed porous high water absorption microballoon, comprising the following steps:
(1) anionic monomer acrylic acid or methacrylic acid are add to deionized water, it is molten with sodium hydroxide under room temperature
Liquid neutralizes, and control degree of neutralization is 55~75%；Nonionic monomer acrylamide, propenyl polyoxyethylene ether, Ji Wusi is then added
Alcohol allyl ether, control monomer mass are anionic monomer: 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, dosage difference
Are as follows: 1~3%, 0.25~1%, 0.01~0.5%, 5~20%；
(3) taking viscosity is the dimethicone of 50~100mPas, and the calcium chloride that mass fraction is 5~15% is then added
Solution；After grease is mutually layered, oil is heated mutually to 60~80 DEG C, is instilled reaction solution and is reacted；Reaction medium be divided into water layer and
Oil reservoir, water layer are calcium chloride solutions, and oil reservoir is dimethicone, and water layer solution pillar height is greater than 5cm.Reaction drop is introduced into water layer
Solidify balling-up, the reaction was continued subsequently into oil reservoir.Size droplet diameter control is 0.5~3mm, and it is thick that final microballoon shell coats a tunic
For 50~300 μm of Calcium alginate films.
(4) after reaction, washing, desciccate, obtain the porous high water absorption microballoon of pearl.
Preferably, the initiator is azo in the preparation method of above-mentioned hud typed porous high water absorption microballoon
The compound of initiator and persulfuric acid salt initiator, wherein azo is two isobutyl imidazole hydrochloride of azo, two isobutyl of azo
Base amidine hydrochloride or azo dicyclohexyl formonitrile HCN.Persulfate is potassium peroxydisulfate or ammonium persulfate, and mass ratio control is azo
Class: persulfuric acid salt=3:1~5:1.
Preferably, the pore-foaming agent is mixed for ternary in the preparation method of above-mentioned hud typed porous high water absorption microballoon
Object is closed, a urmaterie is one or both of sodium bicarbonate, saleratus；Binary substance is urea；Ternary materials are ethyl alcohol
With the compound of one or both of acetone；The mass ratio control of ternary materials is 1:3:2 or 1:3:1 or 1:2:2 or 1:2:
3.One Ying Keyu carboxyl reacts or itself can decompose generation gas, and one needs and water generated reactive gas at 100 DEG C or so,
One should be easy to volatilize and not with monomer reaction.
Preferably, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, dry temperature described in step (4)
Degree is 80~100 DEG C, and drying time is 6~8h.
Preferably, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, while adding pore-foaming agent,
Also add coloring agent, aromatic, fertilizer or magnetisable material.
Preferably, the crosslinking agent is polynary alkene in the preparation method of above-mentioned hud typed porous high water absorption microballoon
One of propyl or diolefin crosslinking agent are a variety of.
Preferably, the polynary allyl is alkene in the preparation method of above-mentioned hud typed porous high water absorption microballoon
Propylated starches, allylation cellulose or tetraallyl oxygroup ethane；The diolefin crosslinking agent is N, N '-di-2-ethylhexylphosphine oxide
Acrylamide.
Be equipped with preferably, in the preparation method of above-mentioned hud typed porous high water absorption microballoon, in reaction vessel can on
The filter vat of lower movement controls residence time of the water suction microballoon in water layer and oil reservoir by controlling the position of filter vat.Instead
After answering, lifts filter vat and collect microballoon, wherein filter vat is made of the sieve of 100 mesh.
Preferably, the reaction solution passes through pore in the preparation method of above-mentioned hud typed porous high water absorption microballoon
Device is added dropwise, and size droplet diameter is 0.5~3mm.
Compared with prior art, the invention has the following beneficial effects:
The present invention is used in combination using a variety of pore-foaming agents, and the pore mechanism of three kinds of pore-foaming agents is different, compared to single cause
The effect of hole agent, the obtained pore structure size reasonable of the present invention, is evenly distributed, can guarantee the quantity of pore structure.The present invention
Complete granulation process before polymerization reaction by the solidification of sodium alginate, and microballoon is formed with certain elasticity after granulation
With the Calcium alginate film of hardness, into oily phase after without by stirring-granulating and will not adhesion it is blocking, therefore do not need using
Suspension stabilizer.Calcium alginate film still keeps certain intensity after microballoon can also be made to absorb water, expand application range.Reaction dress
Middle installation filter vat is set, can directly lift filter vat after reaction and collect product, it is easy to operate and safe.
Detailed description of the invention
Fig. 1 is the schematic diagram of pore dropper.
1 is feed opening, and 2 be nitrogen inlet, and 3 be capillary or the tubule with thin mouth nozzle, and 4 be filter vat, and 5 be 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 that whether there is or not the microballoon aspect graphs of cured layer.
Specific embodiment
Embodiment 1:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 65% that 30% sodium hydroxide solution (sodium hydroxide 26g+ deionized water 60.67g), which is neutralized to degree of neutralization,.Then 24.02g is added
Acrylamide.
(2) liquid to be neutralized is cooled to room temperature, and sequentially adds sodium alginate: 1g, tetraallyl oxygroup ethane: 0.48g, azo
Two isobutyl imidazole hydrochlorides: 0.2g, potassium peroxydisulfate: 0.025g, sodium bicarbonate: 1.6g, urea: 4.8g, ethyl alcohol: 3.2g.Mixing
It is uniformly spare.
(3) taking 300g viscosity is the dimethicone of 50mPas, and the calcium chloride solution that 100g mass fraction is 5% is delayed
Slowly it pours into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lifted
Lauter tub collects product, is washed three times with ethyl acetate, is then placed into 85 DEG C of constant temperature blast drying oven dry 8h, final to obtain
To hud typed porous water-absorbing microballoon.The schematic diagram of pore dropper is as shown in Figure 1,1 is feed opening, and 2 be nitrogen inlet, and 3 are
Capillary or tubule with thin mouth nozzle, 4 be filter vat, and 5 be removable adjuster.Gained absorb water microballoon core-shell structure with
Pore structure is shown in that Fig. 2, the metallurgical microscopic and SEM of microballoon a quarter section scheme, and shell thickness is about thick 1/10 of core.Before and after pore,
Microballoon rate of water absorption, which compares, sees Fig. 3.Whether there is or not the microballoon forms of cured layer to see Fig. 4.
Embodiment 2:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 70% that 30% sodium hydroxide solution (sodium hydroxide 28g+ deionized water 65.33g), which is neutralized to degree of neutralization,.Then 18.02g is added
Propenyl polyoxyethylene ether.
(2) liquid to be neutralized is cooled to room temperature, and sequentially adds sodium alginate: 1.5g, tetraallyl oxygroup ethane: 0.24g, N,
N '-methylene-bisacrylamide: 0.24g, two isobutyl imidazole hydrochloride of azo: 0.2g, ammonium persulfate: 0.025g, bicarbonate
Potassium: 1.6g, urea: 4.8g, acetone: 3.2g.It is uniformly mixed spare.
(3) taking 300g viscosity is the dimethicone of 50mPas, and the calcium chloride solution that 100g mass fraction is 7% is delayed
Slowly it pours into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lifted
Lauter tub collects product, is washed three times with ethyl acetate, is then placed into 85 DEG C of constant temperature blast drying oven dry 8h, final to obtain
To hud typed porous water-absorbing microballoon.
Embodiment 3:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 75% that 30% sodium hydroxide solution (sodium hydroxide 30g+ deionized water 100g), which is neutralized to degree of neutralization,.Then 18.02g season is added
Penta tetrol allyl ether.
(2) liquid to be neutralized is cooled to room temperature, and sequentially adds sodium alginate: 2g, allylation starch: 0.48g, azo two are different
Butyl Amidine HCl salt: 0.2g, potassium peroxydisulfate: 0.05g, saleratus: 1.6g, urea: 4.8g, acetone: 1.6g, ethyl alcohol: 1.6g.
It is uniformly mixed spare.
(3) taking 300g viscosity is the dimethicone of 50mPas, and the calcium chloride solution that 100g mass fraction is 9% is delayed
Slowly it pours into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lifted
Lauter tub collects product, is washed three times with ethyl acetate, is then placed into 85 DEG C of constant temperature blast drying oven dry 8h, final to obtain
To hud typed porous water-absorbing microballoon.
Embodiment 4:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 70% that 30% sodium hydroxide solution (sodium hydroxide 28g+ deionized water 65.33g), which is neutralized to degree of neutralization,.Then 18.02g is added
Acrylamide, 6g pentaerythrite allyl ether.
(2) liquid to be neutralized is cooled to room temperature, and 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 bicarbonate:
1.6g, urea: 4.8g, ethyl alcohol: 1.6g.It is uniformly mixed spare.
(3) taking 300g viscosity is the dimethicone of 100mPas, the calcium chloride solution for being 11% by 100g mass fraction
It is poured slowly into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lift
Filter vat collects product, is washed three times with ethyl acetate, is then placed into 85 DEG C of constant temperature blast drying oven dry 8h, finally
Obtain hud typed porous water-absorbing microballoon.
Embodiment 5:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 70% that 30% sodium hydroxide solution (sodium hydroxide 28g+ deionized water 65.33g), which is neutralized to degree of neutralization,.Then 12.01g is added
Acrylamide, 12.01g propenyl polyoxyethylene ether.
(2) liquid to be neutralized is cooled to room temperature, and 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, ethyl alcohol: 0.8g, acetone:
0.8g.It is uniformly mixed spare.
(3) taking 200g viscosity is the dimethicone of 100mPas, the calcium chloride solution for being 13% by 100g mass fraction
It is poured slowly into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lift
Filter vat collects product, is washed three times with ethyl acetate, is then placed into 100 DEG C of constant temperature blast drying oven dry 8h, most
Hud typed porous water-absorbing microballoon is obtained eventually.
Embodiment 6:
(1) 72.06g acrylic acid is added in 38.88g deionized water, is uniformly mixed, is with mass fraction under room temperature
It is 70% that 30% sodium hydroxide solution (sodium hydroxide 28g+ deionized water 65.33g), which is neutralized to degree of neutralization,.Then 8.01g is added
Acrylamide, 8.01g propenyl polyoxyethylene ether, 8.01g pentaerythrite allyl ether.
(2) liquid to be neutralized is cooled to room temperature, and 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 bicarbonate:
0.8g, saleratus: 0.8g, urea: 4.8g, ethyl alcohol: 1.6g, acetone: 1.6g.It is uniformly mixed spare.
(3) taking 200g viscosity is the dimethicone of 100mPas, the calcium chloride solution for being 15% by 100g mass fraction
It is poured slowly into dimethicone.After grease layering, oil is heated mutually to 70 DEG C, reaction solution is added dropwise.After reaction, lift
Filter vat collects product, is washed three times with ethyl acetate, is then placed into 100 DEG C of constant temperature blast drying oven dry 8h, most
Hud typed porous water-absorbing microballoon is obtained eventually.
Claims (8)
1. a kind of preparation method of hud typed porous high water absorption microballoon, it is characterised in that the following steps are included:
(1) anionic monomer acrylic acid or methacrylic acid are add to deionized water, in sodium hydroxide solution under room temperature
With, control degree of neutralization be 55~75%；Nonionic monomer acrylamide, propenyl polyoxyethylene ether or pentaerythrite is then added
Allyl ether, control monomer mass are anionic monomer: 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, dosage is respectively as follows: 1
~3%, 0.25~1%, 0.01~0.5%, 5~20%；
(3) taking viscosity is the dimethicone of 50~100mPas, and it is molten that the calcium chloride that mass fraction is 5~15% is then added
Liquid；After grease is mutually layered, oil is heated mutually to 60~80 DEG C, is instilled reaction solution and is reacted；It is solid that reaction drop is introduced into water layer
It is melted into ball, the reaction was continued subsequently into oil reservoir；
(4) after reaction, washing, desciccate, obtain the porous high water absorption microballoon of pearl；
The pore-foaming agent is ternary mixture, and a urmaterie is one or both of sodium bicarbonate, saleratus；Binary substance
For urea；Ternary materials are the compound of one or both of ethyl alcohol and acetone；The mass ratio control of ternary materials is 1:3:2
Or 1:3:1 or 1:2:2 or 1:2:3.
2. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that the initiator is
The compound of azo-initiator and persulfuric acid salt initiator, wherein azo is two isobutyl imidazole hydrochloride of azo, azo
Diisobutyl amidine hydrochloride or azo dicyclohexyl formonitrile HCN, persulfate are potassium peroxydisulfate or ammonium persulfate, mass ratio control
For azo: persulfuric acid salt=3:1~5:1.
3. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that step (4) is described
Drying temperature be 80~100 DEG C, drying time be 6~8h.
4. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that in addition pore-foaming agent
While, also add coloring agent, aromatic, fertilizer or magnetisable material.
5. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that the crosslinking agent is
One of polynary allyl or diolefin crosslinking agent are a variety of；
The polynary allyl is allylation starch, allylation cellulose or tetraallyl oxygroup ethane；The diolefin
Crosslinking agent is N, N '-methylene-bisacrylamide.
6. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that set in reaction vessel
Have filter vat moving up and down, after reaction, by filter vat collect microballoon, filter vat bottom surface by 100 mesh sieve system
At.
7. the preparation method of hud typed porous high water absorption microballoon according to claim 1, which is characterized in that the reaction solution is logical
It crosses pore dropper to be added dropwise, size droplet diameter is 0.5~3mm.
8. a kind of hud typed porous high water absorption microballoon, it is characterised in that prepared by the described in any item methods of claim 1~7
It obtains.
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| CN107815447B (en) * | 2017-12-11 | 2021-09-14 | 杭州富阳佳畅机械有限公司 | Immobilized composite algae microspheres and application thereof |
| CN107827328B (en) * | 2017-12-14 | 2021-03-05 | 杭州富阳佳畅机械有限公司 | Process for repairing aquaculture wastewater |
| CN107935189B (en) * | 2017-12-14 | 2020-12-22 | 杭州富阳佳畅机械有限公司 | Process for treating domestic sewage by using algae microspheres |
| CN111718438A (en) * | 2019-03-20 | 2020-09-29 | 华东理工大学 | Preparation method of porous sodium polyacrylate super absorbent resin |
| CN114790264B (en) * | 2022-05-12 | 2024-04-05 | 兰州理工大学 | Spherical gel particles and preparation method and application thereof |
| 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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