CN104841386A - Preparation method for composite high oil-absorption resin - Google Patents
Preparation method for composite high oil-absorption resin Download PDFInfo
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Abstract
Relating to the high oil-absorption resin preparation field, the invention discloses a preparation method for a composite high oil-absorption resin. The method includes: (1) preparation of immobilized microbial microspheres: mixing modified mussel shell powder with a seed bacterial liquid, adding a sodium alginate solution into a bacteria adsorbing modified mussel shell powder solution, then injecting the mixed solution into a calcium chloride solution and conducting dispersion into balls, and conducting crosslinking to obtain immobilized microbial microspheres; (2) preparation of an acrylate copolymer emulsion: adding a methylacrylate monomer, styrene, an initiator and an emulsifier into water and conducting stirring emulsification; adding a crosslinking agent and a pore making agent into the emulsion to carry out reaction so as to obtain an acrylate copolymer emulsion; and (3) preparation of composite high oil-absorption resin: adding immobilized microbial microspheres, a coupling agent and cellulose into the acrylate copolymer emulsion, conducting stirring and then performing vacuum drying, thus obtaining the composite high oil-absorption resin. The composite high oil-absorption resin prepared by the method provided by the invention has fast oil absorption speed and large oil absorption capacity, and can carry out microbial degradation on oil.
Description
Technical field
The present invention relates to high oil-absorbing resin preparation field, particularly relate to a kind of preparation method of compound high oil-absorbing resin.
Background technology
Come in the past few decades, the fast development of the industry of China, national life level also improves constantly, but along with industrial expansion, industry is also more and more serious to the pollution of environment.In recent years, the environmental consciousness of people is strengthened gradually, and government also more and more payes attention to for environmental improvement.
In numerous pollution source, water pollution problems is particularly outstanding, wherein, the leakage of industry oil causes huge pollution with discharge to ocean, river, the serious threat to environment structure.
At present, the general oil absorption material that adopts adsorbs the oil in water body, and what use at most is high oil-absorbing resin.High oil-absorbing resin is the monomer crosslinked polymer of lipophile, and intermolecular have three-dimensional crosslinked network shape structure, makes resin generation swelling action by the solvation of Intramolecular oil base segment and oil molecule.Can not dissolve because high oil-absorbing resin can only occur swelling, therefore oil molecule will be carried in tridimensional network, realizes high oil-absorbing resin oil suction and protects oily function.
The swelling rate of high oil-absorbing resin is high, Oil keeping is good, but after high oil-absorbing resin adsorbed oil molecule reaches capacity, need to carry out separation and recovery to oil, because the Oil keeping of high oil-absorbing resin is good, oil is difficult to reclaim by after high oil-absorbing resin absorption, and current separation and recovery technology energy consumption is high, complicated operation, cost is high.
Summary of the invention
In order to solve in prior art after high oil-absorbing resin oil suction the technical problem of oily difficult separation and recycling, the invention provides a kind of preparation method of compound high oil-absorbing resin, compound high oil-absorbing resin swelling rate prepared by the method is fast, oil absorption is large, and microbial degradation can be carried out to by the oil after adsorbing, make high oil-absorbing resin can remove greasy dirt in water body long-term effectively.
Concrete technical scheme of the present invention is: a kind of preparation method of compound high oil-absorbing resin, and concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Get 10 parts of modification mussel shell powder and 20-50 part petroleum hydrocarbon degradation bacteria concentration is 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria.
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 4-8wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 2.5wt-3.5wt%, obtained immobilized microorganism microballoon after crosslinked 6-18h.
When mixed solution is injected into calcium chloride solution, to be injected in calcium chloride solution, calcium chloride slowly enters microballoon with spherical for sodium alginate and modification mussel shell powder, and is fixed in microballoon after forming calcium alginate with sodium alginate.
(2) preparation of acrylate copolymer emulsion:
Get 65-85 part methacrylate-based monomer, 20-30 part styrene, 0.5-1.5 part initator, 3-7 part emulsifying agent join stirring and emulsifying 1-2h in 250-450 part water, obtain emulsion.
Add 3-5 part crosslinking agent, 45-55 part perforating agent in above-mentioned emulsion after, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 65-85 DEG C, and the reaction time is 4-8h, obtains acrylate copolymer emulsion after reaction terminates.
(3) preparation of compound high oil-absorbing resin:
Getting the above-mentioned immobilized microorganism microballoon of 5-20 part, 0.1-0.5 part coupling agent and 1-5 part cellulose joins in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures.
In above-mentioned compound high oil-absorbing resin, due to the existence of perforating agent, resin inside is made to have a large amount of fine pore passage structures, resin is made to have fast absorbing oil ability and larger oil tankage, cellulosic compound further enhances the oil absorption of resin, enhances the toughness of resin simultaneously; And immobilized microorganism micro-ball load is in resin, there is stronger stability, simultaneously due to be under normal temperature stirring at low speed condition with acrylate copolymer emulsion compound, polymeric inner network structure formation condition is comparatively gentle, farthest guarantees that microbial cell is without prejudice.
Each component score is parts by weight above.
Further, described in step (1), the preparation method of modification mussel shell powder is:
Got 40-80 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 1-2h, the weight consumption of described mussel shell powder and citric acid is than being 1:1-3.
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 400-600 DEG C, takes out after 0.5-1h and obtain thermal activation mussel shell powder.
Modification mussel shell powder was obtained after above-mentioned thermal activation mussel shell powder is pulverized 150-200 order.
Its adsorption capacity modified carried out to mussel shell powder stronger.
Further, methacrylate-based monomer described in step (2) is selected from least one in lauryl methacrylate, methacrylic acid 13 ester, and methyl methacrylate, EMA, at least one in butyl methacrylate.
Further, emulsifying agent described in step (2) is neopelex, described initator is persulfate, described crosslinking agent is N, N '-methylene-bisacrylamide, described perforating agent be ethyl acetate.
Further, described in step (3), coupling agent is silane coupler.
Further, together join the nano titanium oxide in addition in described acrylate copolymer emulsion in step (3) with described immobilized microorganism microballoon, coupling agent and cellulose, the consumption of described part nano titanium oxide is 1-5 part.
Adding of nano titanium oxide, resin is made to have stronger ageing resistance, particularly anti-uv-ray; because for process rivers; particularly during deepwater oil slick, usually can suffer long Exposure to Sunlight, improve the physical life that anti-light aging ability contributes to extending resin.
Further, the particle diameter of described nano titanium oxide is 10-50 nanometer.
Further, the petroleum hydrocarbon degradation bacterium described in step (1) is bacillus brevis D-1.
Be compared with the prior art, the invention has the beneficial effects as follows: the fine pore passage structure of compound high oil-absorbing resin inside prepared by the present invention is numerous, has swelling rate, larger absorbency capacity and outstanding Oil keeping fast.Inside is compounded with immobilized microorganism simultaneously, the oil being absorbed into resin inside can be decomposed, immobilized microorganism with modification mussel shell powder-sodium alginate-calcium chloride for carrier, to the good stability of microorganism solidification, and modification mussel shell powder has loose structure, also there is good adsorptivity, nutriment can be made more easily by microorganism panning, improve survival rate and the activity of microorganism, degradation efficiency is high.This compound high oil-absorbing resin by the oily disintegrate of absorption, can carry out oil suction and oil degraded, without the need to carrying out separation and recovery simultaneously.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A preparation method for compound high oil-absorbing resin, concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Got 60 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 1.5h, the weight consumption of described mussel shell powder and citric acid is than being 1:2.
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 500 DEG C, takes out after 1h and obtain thermal activation mussel shell powder, after thermal activation mussel shell powder is pulverized 200 orders, obtained modification mussel shell powder.
Get 10 parts of above-mentioned modification mussel shell powder and 35 parts of bacillus brevis D-1 concentration are 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria.
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 6wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 3wt%, obtained immobilized microorganism microballoon after crosslinked 12h.
(2) preparation of acrylate copolymer emulsion:
Get 50 parts of lauryl methacrylate, 25 parts of methyl methacrylates, 25 parts of styrene, 1 part of potassium peroxydisulfate, 5 parts of neopelexes join stirring and emulsifying 2h in 350 parts of water, obtain emulsion.
In above-mentioned emulsion, after interpolation 4 parts of N, N '-methylene-bisacrylamide, 50 parts of ethyl acetate, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 75 DEG C, and the reaction time is 6h, obtains acrylate copolymer emulsion after reaction terminates.
(3) preparation of compound high oil-absorbing resin:
Getting 15 parts of above-mentioned immobilized microorganism microballoons, 0.3 part of silane coupler and 3 parts of celluloses joins in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
Embodiment 2
A preparation method for compound high oil-absorbing resin, concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Got 80 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 1h, the weight consumption of described mussel shell powder and citric acid is than being 1:3.
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 600 DEG C, takes out after 0.5h and obtain thermal activation mussel shell powder, after thermal activation mussel shell powder is pulverized 150 orders, obtained modification mussel shell powder.
Get 10 parts of above-mentioned modification mussel shell powder and 50 parts of bacillus brevis D-1 concentration are 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria.
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 4.5wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 2.5wt%, obtained immobilized microorganism microballoon after crosslinked 18h.
When mixed solution is injected into calcium chloride solution, to be injected in calcium chloride solution, calcium chloride slowly enters microballoon with spherical for sodium alginate and modification mussel shell powder, and is fixed in microballoon after forming calcium alginate with sodium alginate.
(2) preparation of acrylate copolymer emulsion:
Get 45 parts of lauryl methacrylate, 20 parts of methyl methacrylates, 20 parts of styrene, 0.5 part of potassium peroxydisulfate, 3 parts of neopelexes join stirring and emulsifying 1h in 450 parts of water, obtain emulsion.
In above-mentioned emulsion, after interpolation 3 parts of N, N '-methylene-bisacrylamide, 45 parts of ethyl acetate, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 65 DEG C, and the reaction time is 8h, obtains acrylate copolymer emulsion after reaction terminates.
(3) preparation of compound high oil-absorbing resin:
Get 20 parts of above-mentioned immobilized microorganism microballoons, nano titanium oxide that 0.5 part of silane coupler, 2 parts of particle diameters are 20 ran and 2 parts of celluloses join in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
Embodiment 3
A preparation method for compound high oil-absorbing resin, concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Got 40 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 2h, the weight consumption of described mussel shell powder and citric acid is than being 1:1.5.
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 450 DEG C, takes out after 1 h and obtain thermal activation mussel shell powder, after thermal activation mussel shell powder is pulverized 200 orders, obtained modification mussel shell powder.
Get 10 parts of above-mentioned modification mussel shell powder and 30 parts of bacillus brevis D-1 concentration are 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria.
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 7.5wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 2.5wt%, obtained immobilized microorganism microballoon after crosslinked 7h.
When mixed solution is injected into calcium chloride solution, to be injected in calcium chloride solution, calcium chloride slowly enters microballoon with spherical for sodium alginate and modification mussel shell powder, and is fixed in microballoon after forming calcium alginate with sodium alginate.
(2) preparation of acrylate copolymer emulsion:
Get 20 parts of lauryl methacrylate, 35 parts of methacrylic acid 13 esters, 25 parts of butyl methacrylates, 20 parts of styrene, 1 part of potassium peroxydisulfate, 6 parts of neopelexes join stirring and emulsifying 2h in 350 parts of water, obtain emulsion.
In above-mentioned emulsion, after interpolation 4 parts of N, N '-methylene-bisacrylamide, 48 parts of ethyl acetate, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 85 DEG C, and the reaction time is 7h, obtains acrylate copolymer emulsion after reaction terminates.
(3) preparation of compound high oil-absorbing resin:
Get 5 parts of above-mentioned immobilized microorganism microballoons, nano titanium oxide that 0.5 part of silane coupler, 5 parts of particle diameters are 40 ran and 5 parts of celluloses join in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
Embodiment 4
A preparation method for compound high oil-absorbing resin, concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Got 80 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 1h, the weight consumption of described mussel shell powder and citric acid is than being 1:1.
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 550 DEG C, takes out after 1 h and obtain thermal activation mussel shell powder, after thermal activation mussel shell powder is pulverized 200 orders, obtained modification mussel shell powder.
Get 10 parts of above-mentioned modification mussel shell powder and 25 parts of bacillus brevis D-1 concentration are 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria.
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 4wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 2.5wt%, obtained immobilized microorganism microballoon after crosslinked 16h.
When mixed solution is injected into calcium chloride solution, to be injected in calcium chloride solution, calcium chloride slowly enters microballoon with spherical for sodium alginate and modification mussel shell powder, and is fixed in microballoon after forming calcium alginate with sodium alginate.
(2) preparation of acrylate copolymer emulsion:
Get 30 parts of lauryl methacrylate, 25 parts of methacrylic acid 13 esters, 30 parts of butyl methacrylates, 30 parts of styrene, 1 part of potassium peroxydisulfate, 7 parts of neopelexes join stirring and emulsifying 2h in 450 parts of water, obtain emulsion.
In above-mentioned emulsion, after interpolation 5 parts of N, N '-methylene-bisacrylamide, 53 parts of ethyl acetate, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 80 DEG C, and the reaction time is 5.5h, obtains acrylate copolymer emulsion after reaction terminates.
(3) preparation of compound high oil-absorbing resin:
Get 20 parts of above-mentioned immobilized microorganism microballoons, nano titanium oxide that 1 part of silane coupler, 3 parts of particle diameters are 40 ran and 3 parts of celluloses join in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure transformation, all still belong to the protection domain of technical solution of the present invention.
Claims (8)
1. a preparation method for compound high oil-absorbing resin, is characterized in that concrete steps are as follows:
(1) preparation of immobilized microorganism microballoon:
Get 10 parts of modification mussel shell powder and 20-50 part petroleum hydrocarbon degradation bacteria concentration is 6 × 10
9the kind daughter bacteria liquid mixing of cell/g, until described modification mussel shell powder adsorbs after described kind of daughter bacteria liquid reaches capacity, obtains the modification mussel shell powder liquid of attracts bacteria;
In the modification mussel shell powder liquid of above-mentioned attracts bacteria, add 1000 parts of concentration is the sodium alginate soln of 4-8wt%, mixed solution is obtained after mixing, then with balling-up equipment, above-mentioned mixed solution being injected into concentration is disperse balling-up in the calcium chloride solution of 2.5wt-3.5wt%, obtained immobilized microorganism microballoon after crosslinked 6-18h;
(2) preparation of acrylate copolymer emulsion:
Get 65-85 part methacrylate-based monomer, 20-30 part styrene, 0.5-1.5 part initator, 3-7 part emulsifying agent join stirring and emulsifying 1-2h in 250-450 part water, obtain emulsion;
Add 3-5 part crosslinking agent, 45-55 part perforating agent in above-mentioned emulsion after, logical nitrogen carries out heated polymerizable reaction, and reaction temperature is 65-85 DEG C, and the reaction time is 4-8h, obtains acrylate copolymer emulsion after reaction terminates;
(3) preparation of compound high oil-absorbing resin:
Getting the above-mentioned immobilized microorganism microballoon of 5-20 part, 0.1-0.5 part coupling agent and 1-5 part cellulose joins in aforesaid propylene acid ester copolymer emulsion, the obtained compound high oil-absorbing resin of stirring at low speed even final vacuum drying at normal temperatures;
Each component score is parts by weight above.
2. the preparation method of compound high oil-absorbing resin according to claim 1, is characterized in that, described in step (1), the preparation method of modification mussel shell powder is:
Got 40-80 order mussel shell powder to join concentration be in the citric acid solution of 3wt% and stirred, and obtaining acid activation mussel shell powder liquid after acid activation 1-2h, the weight consumption of described mussel shell powder and citric acid is than being 1:1-3;
Above-mentioned acid activation mussel shell powder liquid is carried out thermal activation at 400-600 DEG C, takes out after 0.5-1h and obtain thermal activation mussel shell powder;
Modification mussel shell powder was obtained after above-mentioned thermal activation mussel shell powder is pulverized 150-200 order.
3. the preparation method of compound high oil-absorbing resin according to claim 1, it is characterized in that, methacrylate-based monomer described in step (2) is selected from least one in lauryl methacrylate, methacrylic acid 13 ester, and methyl methacrylate, EMA, at least one in butyl methacrylate.
4. the preparation method of compound high oil-absorbing resin according to claim 1, it is characterized in that, emulsifying agent described in step (2) is neopelex, described initator is persulfate, described crosslinking agent is N, N '-methylene-bisacrylamide, described perforating agent be ethyl acetate.
5. the preparation method of compound high oil-absorbing resin according to claim 1, is characterized in that, described in step (3), coupling agent is silane coupler.
6. the preparation method of compound high oil-absorbing resin according to claim 1, it is characterized in that, together join the nano titanium oxide in addition in described acrylate copolymer emulsion in step (3) with described immobilized microorganism microballoon, coupling agent and cellulose, the consumption of described part nano titanium oxide is 1-5 part.
7. the preparation method of compound high oil-absorbing resin according to claim 6, is characterized in that, the particle diameter of described nano titanium oxide is 10-50 nanometer.
8. the preparation method of compound high oil-absorbing resin according to claim 1, is characterized in that, the petroleum hydrocarbon degradation bacterium described in step (1) is bacillus brevis D-1.
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| CN107837795A (en) * | 2017-11-17 | 2018-03-27 | 浙江海洋大学 | A kind of resin sorbent and preparation method of the load of microorganisms type of degradable greasy dirt |
| CN108546662A (en) * | 2018-05-07 | 2018-09-18 | 中国海洋大学 | Using the method for nitrifying bacteria community-bacillus Combined Treatment breeding wastewater of immobilization respectively |
| CN108753064A (en) * | 2018-06-19 | 2018-11-06 | 广东优爱宝新材料科技有限公司 | A kind of liquid shell powder paint and preparation method thereof |
| CN108993440A (en) * | 2018-06-28 | 2018-12-14 | 奚正华 | It is a kind of for adsorbing the preparation method of the oil-absorbing resin ball of ocean oil slick |
| CN109046291A (en) * | 2018-09-12 | 2018-12-21 | 潘钕 | The preparation method of resin sorbent based on compound diatomite |
| EP3718624A1 (en) * | 2019-04-02 | 2020-10-07 | Acon-Holding Inc. | Composite shell particle, biological material, and method of manufacturing composite shell particle |
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| CN107837795B (en) * | 2017-11-17 | 2020-08-14 | 浙江海洋大学 | Microbial-loaded resin adsorbent capable of degrading oil stains and preparation method thereof |
| CN108546662A (en) * | 2018-05-07 | 2018-09-18 | 中国海洋大学 | Using the method for nitrifying bacteria community-bacillus Combined Treatment breeding wastewater of immobilization respectively |
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| CN108993440A (en) * | 2018-06-28 | 2018-12-14 | 奚正华 | It is a kind of for adsorbing the preparation method of the oil-absorbing resin ball of ocean oil slick |
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| CN109046291A (en) * | 2018-09-12 | 2018-12-21 | 潘钕 | The preparation method of resin sorbent based on compound diatomite |
| EP3718624A1 (en) * | 2019-04-02 | 2020-10-07 | Acon-Holding Inc. | Composite shell particle, biological material, and method of manufacturing composite shell particle |
| US10876093B2 (en) | 2019-04-02 | 2020-12-29 | Acon-Holding Inc. | Composite shell particle, biological material, and method of manufacturing composite shell particle |
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