CN104841388A - Preparation method for resin adsorbent compounded with mussel shell powder - Google Patents
Preparation method for resin adsorbent compounded with mussel shell powder Download PDFInfo
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Abstract
Relating to the resin adsorbent preparation field, the invention discloses a preparation method for a resin adsorbent compounded with mussel shell powder. The method includes: (1) preparation of mussel shell powder immobilized microbial granules: adding a sodium alginate solution into a bacteria adsorbing modified mussel shell powder solution, injecting the mixed solution into a calcium chloride solution to prepare mussel shell powder immobilized microbial granules; (2) preparation of an acrylate copolymer emulsion: adding a methyl acrylate 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, thus obtaining an acrylate copolymer emulsion; and (3) preparation of the resin adsorbent compounded with mussel shell powder: adding the mussel shell powder immobilized microbial granules and a coupling agent into the acrylate copolymer emulsion, and carrying out reaction to obtain the resin adsorbent compounded with mussel shell powder. The resin adsorbent prepared by the method provided by the invention has fast oil absorption rate and large oil absorption capacity, and can perform microbial degradation on oil.
Description
Technical field
The present invention relates to resin sorbent preparation field, particularly relate to a kind of preparation method being compounded with the resin sorbent of mussel shell powder.
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 being compounded with the resin sorbent of mussel shell powder, resin sorbent 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 resin sorbent can remove greasy dirt in water body long-term effectively.
Concrete technical scheme of the present invention is: a kind of preparation method being compounded with the resin sorbent of mussel shell powder, and concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 2.5wt-3.5wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 4-12h.
(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 the resin sorbent of mussel shell powder is compounded with:
Get 5-20 part above-mentioned mussel shell powder immobilization microorganism particles, 0.1-0.5 part coupling agent joins in aforesaid propylene acid ester copolymer emulsion, at normal temperatures the obtained resin sorbent being compounded with mussel shell powder of stirring at low speed even final vacuum drying.
Each component score is parts by weight above.
When mixed solution is injected into calcium chloride solution, after calcium chloride and sodium alginate form calcium alginate, form microorganism carrier with modification mussel shell powder.
Be compounded with in the resin sorbent of mussel shell powder above-mentioned, due to the existence of perforating agent, make resin inside have a large amount of fine pore passage structures, make resin have fast absorbing oil ability and larger oil tankage; And mussel shell powder immobilization microorganism particles is carried 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.
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 mussel shell powder immobilization microorganism particles, coupling agent, 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 prepared by the present invention the be compounded with resin sorbent inside of mussel shell powder 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, mussel shell powder can also also have adsorption capacity to the heavy metal etc. in water body on the other hand, can purifying water body further, mussel shell powder is compound to after in resin, also the mechanical property of resin can be increased.Originally the resin sorbent being compounded with mussel shell powder 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
Be compounded with a preparation method for the resin sorbent of mussel shell powder, concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 3wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 8h.
(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 the resin sorbent of mussel shell powder is compounded with:
Get 15 parts of above-mentioned mussel shell powder immobilization microorganism particles, 0.3 part of silane coupler joins in aforesaid propylene acid ester copolymer emulsion, at normal temperatures the obtained resin sorbent being compounded with mussel shell powder of stirring at low speed even final vacuum drying.
Each component score is parts by weight above.
Embodiment 2
Be compounded with a preparation method for the resin sorbent of mussel shell powder, concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 2.5wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 12h.
(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 the resin sorbent of mussel shell powder is compounded with:
Get 20 parts of above-mentioned mussel shell powder immobilization microorganism particles, nano titanium oxide that 0.5 part of silane coupler, 2 parts of particle diameters are 20 ran joins in aforesaid propylene acid ester copolymer emulsion, the obtained resin sorbent being compounded with mussel shell powder of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
Embodiment 3
Be compounded with a preparation method for the resin sorbent of mussel shell powder, concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 2.5wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 4h.
(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 the resin sorbent of mussel shell powder is compounded with:
Get 5 parts of above-mentioned mussel shell powder immobilization microorganism particles, nano titanium oxide that 0.5 part of silane coupler, 5 parts of particle diameters are 40 ran joins in aforesaid propylene acid ester copolymer emulsion, the obtained resin sorbent being compounded with mussel shell powder of stirring at low speed even final vacuum drying at normal temperatures.
Each component score is parts by weight above.
Embodiment 4
Be compounded with a preparation method for the resin sorbent of mussel shell powder, concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 2.5wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 6h.
(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) resin sorbent of mussel shell powder is compounded with:
Get 20 parts of above-mentioned mussel shell powder immobilization microorganism particles, nano titanium oxide that 1 part of silane coupler, 3 parts of particle diameters are 40 ran joins in aforesaid propylene acid ester copolymer emulsion, the obtained resin sorbent being compounded with mussel shell powder 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. be compounded with a preparation method for the resin sorbent of mussel shell powder, it is characterized in that concrete steps are as follows:
(1) preparation of mussel shell powder immobilization microorganism particles:
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 above-mentioned mixed solution being injected into concentration is in the calcium chloride solution of 2.5wt-3.5wt%, obtained mussel shell powder immobilization microorganism particles after crosslinked 4-12h;
(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 the resin sorbent of mussel shell powder is compounded with:
Get 5-20 part above-mentioned mussel shell powder immobilization microorganism particles, 0.1-0.5 part coupling agent joins in aforesaid propylene acid ester copolymer emulsion, at normal temperatures the obtained resin sorbent being compounded with mussel shell powder of stirring at low speed even final vacuum drying;
Each component score is parts by weight above.
2. the preparation method being compounded with the resin sorbent of mussel shell powder 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 being compounded with the resin sorbent of mussel shell powder 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 being compounded with the resin sorbent of mussel shell powder 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 being compounded with the resin sorbent of mussel shell powder according to claim 1, is characterized in that, described in step (3), coupling agent is silane coupler.
6. the preparation method being compounded with the resin sorbent of mussel shell powder 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 mussel shell powder immobilization microorganism particles, coupling agent, the consumption of described part nano titanium oxide is 1-5 part.
7. the preparation method being compounded with the resin sorbent of mussel shell powder according to claim 6, is characterized in that, the particle diameter of described nano titanium oxide is 10-50 nanometer.
8. the preparation method being compounded with the resin sorbent of mussel shell powder 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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| CN105817194A (en) * | 2015-12-15 | 2016-08-03 | 浙江海洋学院 | Preparation method for recoverable adsorption microsphere for oil stains on sea surface |
| CN105903432A (en) * | 2016-05-16 | 2016-08-31 | 无锡摩顶科技有限公司 | Waste water dephosphorization absorption material, and preparation method and application thereof |
| CN107583618A (en) * | 2017-09-27 | 2018-01-16 | 浙江海洋大学 | A kind of sodium alginate/mussel shell powder microballoon and application thereof |
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Application publication date: 20150819 |