CN109133330A - A kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material - Google Patents
A kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material Download PDFInfo
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- CN109133330A CN109133330A CN201811014692.XA CN201811014692A CN109133330A CN 109133330 A CN109133330 A CN 109133330A CN 201811014692 A CN201811014692 A CN 201811014692A CN 109133330 A CN109133330 A CN 109133330A
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- polypropylene
- dosage form
- packing material
- biologic packing
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- 239000000463 material Substances 0.000 title claims abstract description 33
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 26
- 239000002552 dosage form Substances 0.000 title claims abstract description 26
- 238000012856 packing Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000499 gel Substances 0.000 claims abstract description 71
- 108010010803 Gelatin Proteins 0.000 claims abstract description 50
- 239000008273 gelatin Substances 0.000 claims abstract description 50
- 229920000159 gelatin Polymers 0.000 claims abstract description 50
- 235000019322 gelatine Nutrition 0.000 claims abstract description 50
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 27
- 229960001631 carbomer Drugs 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 26
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 24
- 230000007071 enzymatic hydrolysis Effects 0.000 claims abstract description 23
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 22
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004014 plasticizer Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002274 desiccant Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010790 dilution Methods 0.000 claims abstract description 16
- 239000012895 dilution Substances 0.000 claims abstract description 16
- 108010059378 Endopeptidases Proteins 0.000 claims abstract description 15
- 102000005593 Endopeptidases Human genes 0.000 claims abstract description 15
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 14
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 102000004190 Enzymes Human genes 0.000 claims abstract description 8
- 108090000790 Enzymes Proteins 0.000 claims abstract description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000009849 deactivation Effects 0.000 claims abstract description 8
- 238000000502 dialysis Methods 0.000 claims abstract description 8
- 238000005453 pelletization Methods 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- ZZMVLMVFYMGSMY-UHFFFAOYSA-N 4-n-(4-methylpentan-2-yl)-1-n-phenylbenzene-1,4-diamine Chemical group C1=CC(NC(C)CC(C)C)=CC=C1NC1=CC=CC=C1 ZZMVLMVFYMGSMY-UHFFFAOYSA-N 0.000 claims description 7
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 7
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 7
- 229940088598 enzyme Drugs 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 3
- 108090000317 Chymotrypsin Proteins 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 229960002376 chymotrypsin Drugs 0.000 claims description 3
- PEJVLWCOQVHCAF-UHFFFAOYSA-N dioctyl oxalate Chemical compound CCCCCCCCOC(=O)C(=O)OCCCCCCCC PEJVLWCOQVHCAF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 150000003462 sulfoxides Chemical class 0.000 claims description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 abstract description 15
- 235000019445 benzyl alcohol Nutrition 0.000 abstract description 5
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract 1
- 239000002585 base Substances 0.000 description 15
- 239000004743 Polypropylene Substances 0.000 description 12
- 229920001155 polypropylene Polymers 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 238000004898 kneading Methods 0.000 description 9
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- 238000007710 freezing Methods 0.000 description 6
- 230000008014 freezing Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000000945 filler Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- -1 Polypropylene Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000009777 vacuum freeze-drying Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 210000000496 pancreas Anatomy 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Substances [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Microbiology (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Biodiversity & Conservation Biology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of polypropylene-base load nano-photo catalytic dosage form biologic packing material, belong to material for water treatment technical field.The present invention mixes butyl titanate with absolute ethyl alcohol and stirring, obtains dilution；Endopeptidase and gelatin solution constant temperature being stirred, enzyme deactivation, obtain enzymatic hydrolysis gelatin solution, carbomer is added dropwise and adjusts pH, dilution is added dropwise, insulation reaction adjusts pH, and it is cooling, it filters, it is dry, obtain desiccant gel block；By desiccant gel block and thionyl chloride constant temperature stirring and dissolving, vacuum distillation is added anhydrous benzyl alcohol reaction, removes supernatant, wash, and dialysis must dry pretreatment gel powder；Acrylic resin is kneaded, dry pretreatment gel powder is added, anti-aging agent and plasticiser continue to be kneaded, and extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.The polypropylene-base load nano-photo catalytic dosage form biologic packing material of technical solution of the present invention preparation has the characteristics that excellent wastewater treatment efficiency.
Description
Technical field
The invention discloses a kind of preparation methods of polypropylene-base load nano-photo catalytic dosage form biologic packing material, belong to Shui Chu
Manage field of material technology.
Background technique
Floating stuffing is mainly used for the pretreatment of drinking water embrane method, and anaerobic waste water, the processing of aerobic embrane method are biological film fluidized bed
Deng, it is special a little with its compared with existing other similar fillers, it is mainly reflected in following several respects:
(1) microorganism is liable to stick to filter material surface and forms biomembrane, and biofilm is rapid；
(2) its special structure is easy to fluidize in full pond, and gas consumption is few, power saves, and has good aqueous energy of ventilating, is easy to raw
The generation of object film with fall off, anaerobism, aerobic tank can be used.Its reasonable specific gravity, can not conglomeration, do not block, not heap
Product, installation is very simple, direct plunges into water body；
(3) due to the unstability on this body structure of filler, make it have greatly it is fluidity, both improve oxygen-transfer efficiency, together
When can improve the mass-transfer efficiency of gas, liquid, solid three-phase again；
(4) floating stuffing density can be in water fluidized state under a certain amount of aeration effect, greatly improve close to 1
The mass-transfer efficiency of dissolved oxygen is conducive to the continuous renewal of biomembrane, promotes the degradation of ammonia nitrogen and organic matter；
(5) it is suitble in the case where not affecting the normal production, by being transformed to existing utility, passes through adjusting with can be convenient
The dispensing of filler is than handling different sewage, to adapt to the variation of different quality.
Polypropylene (PP) is a kind of thermoplastic resin as prepared by propylene polymerization.Polypropylene is nontoxic, tasteless, and density is small,
Intensity, rigidity, hardness, heat resistance are preferable, and common acid, alkali organic solvent almost do not work to it.Polypropylene abundance,
It is cheap, it is one of most widely used five big general-purpose plastics, in household electrical appliance, auto industry, agricultural facility, machinery and builds
It builds in equal fields and is widely used.
However, generally can have the inorganic of photocatalysis efficiency by adding to further increase the performance of biofilter material
Catalyst, such as TiO2, and PP is macromolecule organic polymer, is coextruded organic catalyst and PP using conventional extrusion processes
Cheng Zhong, there are the organic catalysts of organic catalyst and PP compatibility and organic catalyst, especially nano-scale in PP base
It being easy to reunite in body, the poor problem of dispersibility can not further increase so as to cause product photocatalysis effect, therefore, how
The inorganic photochemical catalyst of nano-scale fine dispersion in PP resin matrix is set to become the art technology urgently to be resolved
One of problem.
Summary of the invention
The present invention solves the technical problem of: it is directed to Conventional nano TiO2- PP composite suspended filler in the preparation,
It is easy to reunite in nano particle PP matrix, dispersibility is poor, lacks so as to cause what product photocatalysis effect can not further increase
Point provides a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material, specific preparation process is as follows:
(1) butyl titanate and dehydrated alcohol 1:5~1:10 in mass ratio are stirred, obtain dilution；
(2) endopeptidase and gelatin solution 1:30~1:50 constant temperature in mass ratio are stirred, heat up enzyme deactivation, enzymatic hydrolysis gelatin solution is obtained,
It keeps the temperature spare；
(3) carbomer is added dropwise into above-mentioned gained enzymatic hydrolysis gelatin solution and adjusts pH to 2.3~2.6, above-mentioned gained dilution is then added dropwise
Liquid, insulated and stirred reaction after liquid to be diluted is added dropwise, is added dropwise urea liquid and adjusts pH to 7.6~7.8, cooling, filter, do
It is dry, obtain desiccant gel block；
(4) by desiccant gel block and thionyl chloride 1:10~1:20 constant temperature stirring and dissolving in mass ratio, chlorination is added in vacuum distillation
1~2 times of sulfoxide volume of anhydrous benzyl alcohol, constant temperature are stirred to react, and remove supernatant, are washed, and dialysis dry, pulverize, obtain dry
Dry pretreatment gel powder；
(5) according to parts by weight, 40~60 parts of acrylic resins are successively taken, dries for 20~30 parts and pre-processes gel powders, 5~8 parts
Anti-aging agent, 5~8 parts of plasticisers, acrylic resin is kneaded, and is subsequently added into dry pretreatment gel powder, anti-aging agent and plasticiser
Continue to be kneaded, extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.
Step (2) endopeptidase is trypsase, any one in chymotrypsin or elastoser.
Step (2) described gelatin solution the preparation method comprises the following steps: gelatin is mixed with water 1:30~1:50 in mass ratio, stand molten
Swollen, heating stirring dissolution obtains gelatin solution.
Step (2) described heat-retaining condition are as follows: temperature is 40~45 DEG C.
Step (3) carbomer is carbomer 930, any one in carbomer 937 or Acritamer 940.
Step (3) drop rate is 3~5mL/min.
Step (5) anti-aging agent is antioxidant 4020, any one in anti-aging agent RD or antioxidant NBC.
Step (5) plasticiser is dioctyl phthalate, ethanedioic acid dioctyl ester or citroflex A-4
In any one.
The beneficial effects of the present invention are:
Technical solution of the present invention contains the collosol structure sensitive to pH in system, after being added in product, near gelatin isoelectric point
When, colloidal sol can be expanded or be shunk with the change of the pH of environment, prepare when deviateing isoelectric point in contraction state
In the process, firstly, the pH to 2.3~2.6 of carbomer regulation system is added dropwise into enzymolysis liquid, so that tetrabutyl titanate hydrolysis is in
Control environment, meanwhile, pH declines around colloidal sol, the protonated amino in colloidal sol, and mutually exclusive with positive charge of the same race, colloidal sol occurs
Expansion, colloidal sol expansion be conducive to generate titanium dioxide be dispersed in colloidal sol, then be added dropwise urea liquid adjust pH to 7.6~
7.8, pH rises around colloidal sol, the carboxylic ions in colloidal sol, and when being now near colloidal sol isoelectric point, colloidal sol is in contraction-like
State, the appearance hole in system at this time, so that the titanium dioxide generated is further dispersed, with around colloidal sol, pH is risen to
7.6~7.8, deviate the isoelectric point of protein, colloidal sol is in swelling state, so that the titanium dioxide generated is fixed in system,
Secondly, by the pH that urea liquid regulation system is added dropwise, so that carbomer carboxylic ions, part carboxylic in carbomer molecular structure
It is mutually exclusive with like charges after base ionization, unfold carbomer strand, and be well dispersed in system, a side
Face effectively avoids nano-titanium dioxide from reuniting, on the other hand, carbomer strand disperse stretching, extension, so that carbomer molecule
Chain easily tangles with gelatin chains, so that the bond strength between nano-titanium dioxide and gelatin is promoted, to increase poly-
Compatibility between allyl resin and titanium dioxide, to further promote the photocatalysis effect of product.
Specific embodiment
Gelatin is placed in No. 1 beaker with water 1:30~1:50 in mass ratio and is mixed, stirs 10~20min with glass bar,
And No. 1 beaker is placed in digital display and is tested the speed in constant temperature blender with magnetic force, it is 80~85 DEG C in temperature, revolving speed is 300~500r/min
Under the conditions of, heating stirring dissolves 30~50min, obtains gelatin solution；By butyl titanate and dehydrated alcohol 1:5~1:10 in mass ratio
It is placed in No. 2 beakers, under the conditions of revolving speed is 300~500r/min, is stirred 30~50min, obtains dilution；By endopeptidase
It is placed in No. 3 beakers with gelatin solution 1:30~1:50 in mass ratio, and No. 3 beakers is placed in digital display and are tested the speed constant temperature blender with magnetic force
In, under the conditions of temperature is 40~45 DEG C, constant temperature is stirred 40~60min, temperature in beaker is then risen to 80~95 DEG C,
In revolving speed be 300~500r/min under the conditions of, 10~20min of enzyme deactivation is cooled to 40 DEG C, obtain enzymatic hydrolysis gelatin solution, in temperature be 40
Under the conditions of~45 DEG C, keep the temperature spare；Carbomer is added dropwise into gained enzymatic hydrolysis gelatin solution and adjusts pH to 2.3~2.6, then with 3~
Above-mentioned gained dilution is added dropwise to gained enzymatic hydrolysis gelatin solution in the rate of 5mL/min, and under the conditions of temperature is 40~45 DEG C, heat preservation is stirred
Mix 40~60min of reaction, after liquid to be diluted is added dropwise, then to after reaction enzymatic hydrolysis gelatin solution be added dropwise mass fraction be 10~
20% urea liquid adjusts pH to 7.6~7.8, and after being cooled to room temperature, filtering obtains gel piece, gel piece is then placed in vacuum
It is dry in freeze drying box, obtain desiccant gel block；Desiccant gel block and thionyl chloride 1:10~1:20 in mass ratio are placed in three
In mouthful flask, and three-necked flask is placed in water-bath, in temperature be 40~45 DEG C, it is permanent under the conditions of revolving speed is 300~500r/min
Temperature stirring is completely dissolved up to desiccant gel block, obtains dissolution mixed liquor, three-necked flask is then connected vacuum plant, be in pressure
40~50kPa, under the conditions of temperature is 40~50 DEG C, the liquid being evaporated under reduced pressure into three-necked flask is completely disappeared, then to three mouthfuls
1~2 times of thionyl chloride volume of anhydrous benzyl alcohol is added in flask, is 40~45 DEG C in temperature, revolving speed is 300~500r/min
Under the conditions of, constant temperature is stirred to react 12~for 24 hours after, remove supernatant, obtain pretreatment gel piece, will then be pre-processed with benzaldehyde
Gel piece washs 2~3 washings, then the pretreatment gel piece after washing is washed 5~8 times with dehydrated alcohol, then will washing
Pretreatment gel piece and distilled water 1:10~1:20 in mass ratio afterwards, which is placed in bag filter, dialyses 4 days, then will be after dialysis
Pretreatment gel piece, which is placed in vacuum freezing drying oven, dry, pulverize, and cross the sieve of 100 mesh, must dry pretreatment gel powder；By weight
Number meter is measured, 40~60 parts of acrylic resins is successively taken, dries for 20~30 parts and pre-process gel powders, 5~8 parts of anti-aging agents, 5~8
Part plasticiser, acrylic resin is placed in kneading machine, under the conditions of temperature is 160~180 DEG C, is kneaded 10~20min, then
Dry pretreatment gel powder is added into kneading machine, anti-aging agent and plasticiser continue to mix under the conditions of temperature is 160~180 DEG C
After refining 30~50min, extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.The endopeptidase is pancreas
Any one in protease, chymotrypsin or elastoser.The carbomer is carbomer 930, carbomer 937 or card wave
Any one in nurse 940.The anti-aging agent is antioxidant 4020, any one in anti-aging agent RD or antioxidant NBC.It is described
Plasticiser is dioctyl phthalate, any one in ethanedioic acid dioctyl ester or citroflex A-4.
Gelatin is placed in No. 1 beaker with water 1:50 in mass ratio and is mixed, stirs 20min with glass bar, and by No. 1 beaker
Digital display is placed in test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 500r/min, heating stirring dissolution
50min obtains gelatin solution；Butyl titanate and dehydrated alcohol 1:10 in mass ratio are placed in No. 2 beakers, in revolving speed be 500r/
Under the conditions of min, it is stirred 50min, obtains dilution；Endopeptidase and gelatin solution 1:50 in mass ratio are placed in No. 3 beakers, and
No. 3 beakers are placed in digital display to test the speed in constant temperature blender with magnetic force, under the conditions of temperature is 45 DEG C, constant temperature is stirred 60min, connects
Temperature in beaker is risen to 95 DEG C, in revolving speed be 500r/min under the conditions of, enzyme deactivation 20min is cooled to 40 DEG C, obtains enzymatic hydrolysis gelatin
Liquid is kept the temperature spare under the conditions of temperature is 45 DEG C；To gained enzymatic hydrolysis gelatin solution in be added dropwise carbomer adjust pH to 2.6, then with
Above-mentioned gained dilution is added dropwise to gained enzymatic hydrolysis gelatin solution in the rate of 5mL/min, and under the conditions of temperature is 45 DEG C, insulated and stirred is anti-
After answering 60min, liquid to be diluted to be added dropwise, it is 20% urea liquid that mass fraction then, which is added dropwise, to the enzymatic hydrolysis gelatin solution after reaction
PH to 7.8 is adjusted, after being cooled to room temperature, filtering obtains gel piece, gel piece is then placed in drying in vacuum freezing drying oven,
Obtain desiccant gel block；Desiccant gel block and thionyl chloride 1:20 in mass ratio are placed in three-necked flask, and three-necked flask is set
It is 45 DEG C in temperature in water-bath, under the conditions of revolving speed is 500r/min, constant temperature stirring is completely dissolved up to desiccant gel block, is obtained
Mixed liquor is dissolved, three-necked flask is then connected into vacuum plant, is that 50kPa is evaporated under reduced pressure under the conditions of temperature is 50 DEG C in pressure
Liquid into three-necked flask completely disappears, and 2 times of thionyl chloride volume of anhydrous benzyl alcohol is then added into three-necked flask, in
Temperature is 45 DEG C, under the conditions of revolving speed is 500r/min, after constant temperature is stirred to react for 24 hours, removes supernatant, obtains pretreatment gel
Block then will pre-process gel piece with benzaldehyde and wash 3 washings, then the pretreatment gel piece after washing will be washed with dehydrated alcohol
It washs 8 times, the pretreatment gel piece after washing is placed in bag filter with distilled water 1:20 in mass ratio then and is dialysed 4 days, then
Pretreatment gel piece after dialysis, which is placed in vacuum freezing drying oven, dry, pulverize, and crosses the sieve of 100 mesh, obtains dry pretreatment
Gel powder；According to parts by weight, 60 parts of acrylic resins, 30 parts of dry pretreatment gel powders, 8 parts of anti-aging agents, 8 parts of modelings are successively taken
Acrylic resin is placed in kneading machine by agent, under the conditions of temperature is 180 DEG C, is kneaded 20min, is then added into kneading machine
Enter dry pretreatment gel powder, anti-aging agent and plasticiser, under the conditions of temperature is 180 DEG C, continues after being kneaded 50min, extrusion is made
Grain loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.The endopeptidase is trypsase.The carbomer is card
Wave nurse 930.The anti-aging agent is antioxidant 4020.The plasticiser is dioctyl phthalate.
Gelatin is placed in No. 1 beaker with water 1:50 in mass ratio and is mixed, stirs 20min with glass bar, and by No. 1 beaker
Digital display is placed in test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 500r/min, heating stirring dissolution
50min obtains gelatin solution；Butyl titanate and dehydrated alcohol 1:10 in mass ratio are placed in No. 2 beakers, in revolving speed be 500r/
Under the conditions of min, it is stirred 50min, obtains dilution；Endopeptidase and gelatin solution 1:50 in mass ratio are placed in No. 3 beakers, and
No. 3 beakers are placed in digital display to test the speed in constant temperature blender with magnetic force, under the conditions of temperature is 45 DEG C, constant temperature is stirred 60min, connects
Temperature in beaker is risen to 95 DEG C, in revolving speed be 500r/min under the conditions of, enzyme deactivation 20min is cooled to 40 DEG C, obtains enzymatic hydrolysis gelatin
Liquid is kept the temperature spare under the conditions of temperature is 45 DEG C；Then above-mentioned institute is added dropwise to gained enzymatic hydrolysis gelatin solution with the rate of 5mL/min
Dilution, under the conditions of temperature is 45 DEG C, insulated and stirred reacts 60min, after liquid to be diluted is added dropwise, then to after reaction
Enzymatic hydrolysis gelatin solution be added dropwise mass fraction be 20% urea liquid adjust pH to 7.8, after being cooled to room temperature, filtering, obtain gel piece,
Then gel piece is placed in drying in vacuum freezing drying oven, obtains desiccant gel block；Desiccant gel block and thionyl chloride are pressed into matter
Amount is placed in three-necked flask than 1:20, and three-necked flask is placed in water-bath, is 45 DEG C in temperature, revolving speed is 500r/min condition
Under, constant temperature stirring is completely dissolved up to desiccant gel block, and dissolution mixed liquor is obtained, three-necked flask is then connected into vacuum plant, in
Pressure is 50kPa, and under the conditions of temperature is 50 DEG C, the liquid being evaporated under reduced pressure into three-necked flask is completely disappeared, and is then burnt to three mouthfuls
2 times of thionyl chloride volume of anhydrous benzyl alcohol is added in bottle, is 45 DEG C in temperature, under the conditions of revolving speed is 500r/min, constant temperature is stirred
After mixing reaction for 24 hours, supernatant is removed, pretreatment gel piece is obtained, pretreatment gel piece is then washed 3 times with benzaldehyde and is washed
Wash, then the pretreatment gel piece after washing washed 8 times with dehydrated alcohol, then by after washing pretreatment gel piece and distillation
Water 1:20 in mass ratio is placed in bag filter and dialyses 4 days, and the pretreatment gel piece after dialysis is then placed in vacuum freeze drying
It dry, pulverize in case, cross the sieve of 100 mesh, pretreatment gel powder must be dried；According to parts by weight, 60 parts of polypropylene trees are successively taken
Acrylic resin is placed in kneading machine, is in temperature by rouge, 30 parts of dry pretreatment gel powders, 8 parts of anti-aging agents, 8 parts of plasticisers
Under the conditions of 180 DEG C, it is kneaded 20min, dry pretreatment gel powder, anti-aging agent and plasticiser, Yu Wen are then added into kneading machine
Under the conditions of degree is 180 DEG C, continue after being kneaded 50min, extruding pelletization is filled out to get polypropylene-base load nano-photo catalytic dosage form biology
Material.The endopeptidase is trypsase.The anti-aging agent is antioxidant 4020.The plasticiser is dioctyl phthalate.
Gelatin is placed in No. 1 beaker with water 1:50 in mass ratio and is mixed, stirs 20min with glass bar, and by No. 1 beaker
Digital display is placed in test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 500r/min, heating stirring dissolution
50min obtains gelatin solution；Butyl titanate and dehydrated alcohol 1:10 in mass ratio are placed in No. 2 beakers, in revolving speed be 500r/
Under the conditions of min, it is stirred 50min, obtains dilution；Endopeptidase and gelatin solution 1:50 in mass ratio are placed in No. 3 beakers, and
No. 3 beakers are placed in digital display to test the speed in constant temperature blender with magnetic force, under the conditions of temperature is 45 DEG C, constant temperature is stirred 60min, connects
Temperature in beaker is risen to 95 DEG C, in revolving speed be 500r/min under the conditions of, enzyme deactivation 20min is cooled to 40 DEG C, obtains enzymatic hydrolysis gelatin
Liquid is kept the temperature spare under the conditions of temperature is 45 DEG C；To gained enzymatic hydrolysis gelatin solution in be added dropwise carbomer adjust pH to 2.6, then with
Above-mentioned gained dilution is added dropwise to gained enzymatic hydrolysis gelatin solution in the rate of 5mL/min, and under the conditions of temperature is 45 DEG C, insulated and stirred is anti-
After answering 60min, liquid to be diluted to be added dropwise, after being cooled to room temperature, filtering obtains gel piece, it is cold that gel piece is then placed in vacuum
Freeze drying in drying box, obtains desiccant gel block；Desiccant gel block and thionyl chloride 1:20 in mass ratio are placed in three-necked flask,
And three-necked flask is placed in water-bath, it is 45 DEG C in temperature, under the conditions of revolving speed is 500r/min, constant temperature stirring is until desiccant gel
Block is completely dissolved, and obtains dissolution mixed liquor, three-necked flask is then connected vacuum plant, is 50kPa in pressure, temperature is 50 DEG C of items
Under part, the liquid being evaporated under reduced pressure into three-necked flask is completely disappeared, and 2 times of thionyl chloride volume are then added into three-necked flask
Anhydrous benzyl alcohol is 45 DEG C in temperature, under the conditions of revolving speed is 500r/min, after constant temperature is stirred to react for 24 hours, removes supernatant,
Gel piece must be pre-processed, then gel piece will be pre-processed with benzaldehyde and wash 3 times and wash, then by the pretreatment gel piece after washing
It is washed 8 times with dehydrated alcohol, is then placed in the pretreatment gel piece after washing in bag filter with distilled water 1:20 in mass ratio
Dialysis 4 days, then the pretreatment gel piece after dialysis, which is placed in vacuum freezing drying oven, dry, pulverize, and cross the sieve of 100 mesh,
Pretreatment gel powder must be dried；According to parts by weight, 60 parts of acrylic resins are successively taken, dries for 30 parts and pre-processes gel powders, 8 parts
Anti-aging agent, 8 parts of plasticisers, acrylic resin is placed in kneading machine, under the conditions of temperature is 180 DEG C, is kneaded 20min, then
Dry pretreatment gel powder is added into kneading machine, anti-aging agent and plasticiser continue to be kneaded under the conditions of temperature is 180 DEG C
After 50min, extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.The endopeptidase is trypsase.
The carbomer is carbomer 930.The anti-aging agent is antioxidant 4020.The plasticiser is dioctyl phthalate.
Gelatin is placed in No. 1 beaker with water 1:50 in mass ratio and is mixed, stirs 20min with glass bar, and by No. 1 beaker
Digital display is placed in test the speed in constant temperature blender with magnetic force, in temperature be 85 DEG C, under the conditions of revolving speed is 500r/min, heating stirring dissolution
50min obtains gelatin solution；Butyl titanate and dehydrated alcohol 1:10 in mass ratio are placed in No. 2 beakers, in revolving speed be 500r/
Under the conditions of min, it is stirred 50min, obtains dilution；Endopeptidase and gelatin solution 1:50 in mass ratio are placed in No. 3 beakers, and
No. 3 beakers are placed in digital display to test the speed in constant temperature blender with magnetic force, under the conditions of temperature is 45 DEG C, constant temperature is stirred 60min, connects
Temperature in beaker is risen to 95 DEG C, in revolving speed be 500r/min under the conditions of, enzyme deactivation 20min is cooled to 40 DEG C, obtains enzymatic hydrolysis gelatin
Liquid is kept the temperature spare under the conditions of temperature is 45 DEG C；To gained enzymatic hydrolysis gelatin solution in be added dropwise carbomer adjust pH to 2.6, then with
Above-mentioned gained dilution is added dropwise to gained enzymatic hydrolysis gelatin solution in the rate of 5mL/min, and under the conditions of temperature is 45 DEG C, insulated and stirred is anti-
After answering 60min, liquid to be diluted to be added dropwise, it is 20% urea liquid that mass fraction then, which is added dropwise, to the enzymatic hydrolysis gelatin solution after reaction
PH to 7.8 is adjusted, after being cooled to room temperature, filtering obtains gel piece, gel piece is then placed in drying in vacuum freezing drying oven,
Obtain desiccant gel block；According to parts by weight, 60 parts of acrylic resins are successively taken, 30 parts of dry pretreatment gel powders, 8 parts anti-old
Agent, 8 parts of plasticisers, acrylic resin is placed in kneading machine, under the conditions of temperature is 180 DEG C, is kneaded 20min, then to mixed
Dry pretreatment gel powder, anti-aging agent and plasticiser are added in mill, under the conditions of temperature is 180 DEG C, continues to be kneaded 50min
Afterwards, extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.The endopeptidase is trypsase.It is described
Carbomer is carbomer 930.The anti-aging agent is antioxidant 4020.The plasticiser is dioctyl phthalate.
Comparative example: the biofilter material of Yixing water treatment filler factory production.
By example 1 to the resulting polypropylene-base of example 4 load nano-photo catalytic dosage form biologic packing material and comparative example product into
Row performance detection, the specific detection method is as follows:
Taking COD content is the micro-polluted water of 10mg/L, is handled using above-mentioned biofilter material it, after detection processing in water
COD content.
The test of COD removal rate is examined by GB11914-89 " measurement-potassium dichromate method of water chemical oxygen demand " standard
It surveys.
Specific testing result is as shown in table 1:
1 polypropylene-base of table loads the specific testing result of nano-photo catalytic dosage form biologic packing material
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| COD/mg/L | 4.1 | 4.5 | 5.6 | 6.7 | 7.2 |
| COD removal rate/% | 0.59 | 0.55 | 0.44 | 0.33 | 0.28 |
By 1 testing result of table it is found that the polypropylene-base of technical solution of the present invention preparation loads nano-photo catalytic dosage form biologic packing material
Have the characteristics that excellent wastewater treatment efficiency, has broad prospects in the development of material for water treatment technology industry.
Claims (8)
1. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material, it is characterised in that specific preparation step
It is as follows:
(1) butyl titanate and dehydrated alcohol 1:5~1:10 in mass ratio are stirred, obtain dilution；
(2) endopeptidase and gelatin solution 1:30~1:50 constant temperature in mass ratio are stirred, heat up enzyme deactivation, enzymatic hydrolysis gelatin solution is obtained,
It keeps the temperature spare；
(3) carbomer is added dropwise into above-mentioned gained enzymatic hydrolysis gelatin solution and adjusts pH to 2.3~2.6, above-mentioned gained dilution is then added dropwise
Liquid, insulated and stirred reaction, after liquid to be diluted is added dropwise, be added dropwise mass fraction be 10~20% urea liquids adjust pH to 7.6~
7.8, it is cooling, it filters, it is dry, obtain desiccant gel block；
(4) by desiccant gel block and thionyl chloride 1:10~1:20 constant temperature stirring and dissolving in mass ratio, chlorination is added in vacuum distillation
1~2 times of sulfoxide volume of anhydrous benzyl alcohol, constant temperature are stirred to react, and remove supernatant, are washed, and dialysis dry, pulverize, obtain dry
Dry pretreatment gel powder；
(5) according to parts by weight, 40~60 parts of acrylic resins are successively taken, dries for 20~30 parts and pre-processes gel powders, 5~8 parts
Anti-aging agent, 5~8 parts of plasticisers, acrylic resin is kneaded, and is subsequently added into dry pretreatment gel powder, anti-aging agent and plasticiser
Continue to be kneaded, extruding pelletization loads nano-photo catalytic dosage form biologic packing material to get polypropylene-base.
2. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (2) endopeptidase is trypsase, any one in chymotrypsin or elastoser.
3. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (2) described gelatin solution the preparation method comprises the following steps: gelatin is mixed with water 1:30~1:50 in mass ratio, stand molten
Swollen, heating stirring dissolution obtains gelatin solution.
4. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (2) described heat-retaining condition are as follows: temperature is 40~45 DEG C.
5. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (3) carbomer is carbomer 930, any one in carbomer 937 or Acritamer 940.
6. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (3) drop rate is 3~5mL/min.
7. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (5) anti-aging agent is antioxidant 4020, any one in anti-aging agent RD or antioxidant NBC.
8. a kind of preparation method of polypropylene-base load nano-photo catalytic dosage form biologic packing material according to claim 1, special
Sign is: step (5) plasticiser is dioctyl phthalate, in ethanedioic acid dioctyl ester or citroflex A-4
Any one.
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