CN114479346A - Broad-spectrum durable antibacterial granular urea formaldehyde molding compound - Google Patents
Broad-spectrum durable antibacterial granular urea formaldehyde molding compound Download PDFInfo
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- CN114479346A CN114479346A CN202210237518.1A CN202210237518A CN114479346A CN 114479346 A CN114479346 A CN 114479346A CN 202210237518 A CN202210237518 A CN 202210237518A CN 114479346 A CN114479346 A CN 114479346A
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- urea
- molding compound
- zinc oxide
- formaldehyde
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- 229920001807 Urea-formaldehyde Polymers 0.000 title claims abstract description 90
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 71
- 238000000465 moulding Methods 0.000 title claims abstract description 66
- 150000001875 compounds Chemical class 0.000 title claims abstract description 65
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 title claims abstract description 64
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 144
- 239000011787 zinc oxide Substances 0.000 claims abstract description 72
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 17
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 17
- 230000002045 lasting effect Effects 0.000 claims abstract description 17
- 239000011256 inorganic filler Substances 0.000 claims abstract description 14
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- 238000004040 coloring Methods 0.000 claims abstract description 13
- 239000000049 pigment Substances 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000314 lubricant Substances 0.000 claims abstract description 11
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 91
- 238000001035 drying Methods 0.000 claims description 47
- 239000000843 powder Substances 0.000 claims description 41
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- 239000002245 particle Substances 0.000 claims description 25
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 24
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- 238000006297 dehydration reaction Methods 0.000 claims description 24
- 239000008187 granular material Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 23
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- 238000000746 purification Methods 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 230000001965 increasing effect Effects 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 6
- VGGLHLAESQEWCR-UHFFFAOYSA-N N-(hydroxymethyl)urea Chemical compound NC(=O)NCO VGGLHLAESQEWCR-UHFFFAOYSA-N 0.000 claims description 4
- 238000007259 addition reaction Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- QUBQYFYWUJJAAK-UHFFFAOYSA-N oxymethurea Chemical compound OCNC(=O)NCO QUBQYFYWUJJAAK-UHFFFAOYSA-N 0.000 claims description 4
- 229950005308 oxymethurea Drugs 0.000 claims description 4
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- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 230000002401 inhibitory effect Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012860 organic pigment Substances 0.000 claims description 3
- 150000003839 salts Chemical group 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000005550 wet granulation Methods 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
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- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- SJLABBVXMDWALA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O SJLABBVXMDWALA-UHFFFAOYSA-N 0.000 claims description 2
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- 238000005070 sampling Methods 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims 1
- 238000012545 processing Methods 0.000 abstract description 10
- 238000009661 fatigue test Methods 0.000 abstract description 3
- 241000588626 Acinetobacter baumannii Species 0.000 abstract 1
- 241000588915 Klebsiella aerogenes Species 0.000 abstract 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 abstract 1
- 229940092559 enterobacter aerogenes Drugs 0.000 abstract 1
- 239000003242 anti bacterial agent Substances 0.000 description 46
- 229910052709 silver Inorganic materials 0.000 description 14
- 239000004332 silver Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 241000894006 Bacteria Species 0.000 description 8
- -1 polyethylene Polymers 0.000 description 8
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 4
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- 239000011701 zinc Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229920002522 Wood fibre Polymers 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229940121375 antifungal agent Drugs 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
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- 229910052725 zinc Inorganic materials 0.000 description 2
- UJBORAMHOAWXLF-UHFFFAOYSA-N 1-(aziridin-1-yl)octadecan-1-one Chemical compound CCCCCCCCCCCCCCCCCC(=O)N1CC1 UJBORAMHOAWXLF-UHFFFAOYSA-N 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- 206010058667 Oral toxicity Diseases 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
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- QKSKPIVNLNLAAV-UHFFFAOYSA-N bis(2-chloroethyl) sulfide Chemical compound ClCCSCCCl QKSKPIVNLNLAAV-UHFFFAOYSA-N 0.000 description 1
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- 239000004566 building material Substances 0.000 description 1
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- 239000004359 castor oil Substances 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
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- CBOQJANXLMLOSS-UHFFFAOYSA-N ethyl vanillin Chemical class CCOC1=CC(C=O)=CC=C1O CBOQJANXLMLOSS-UHFFFAOYSA-N 0.000 description 1
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- 235000013305 food Nutrition 0.000 description 1
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- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical group COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
- 235000012141 vanillin Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic and acyclic or carbocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a broad-spectrum lasting antibacterial granular urea formaldehyde molding compound which comprises the following components in parts by weight: 1000-1200 parts of urea, 2000-2600 parts of formaldehyde, 40-120 parts of melamine, 18-45 parts of tetrapod-like zinc oxide whiskers, 80-120 parts of hexamethylenetetramine, 20-30 parts of a curing agent, 30-90 parts of an inorganic filler, 540-648 parts of wood pulp (wood pulp), 15-20 parts of a lubricant, 16-20 parts of titanium dioxide and 1.5-2.2 parts of a coloring pigment. After a cold and hot fatigue test, the broad-spectrum lasting antibacterial granular urea-formaldehyde molding compound product has the antibacterial rate of more than 99.99 percent for pseudomonas aeruginosa, acinetobacter baumannii, enterobacter aerogenes and the like, the antibacterial activity value is more than 5.4, and the processing performance and the mechanical strength are improved.
Description
Technical Field
The invention relates to a urea formaldehyde molding compound, in particular to a granular urea formaldehyde molding compound added with four-needle-shaped zinc oxide whiskers
Technical Field
Urea-formaldehyde molding compound (commonly called jade powder) is produced for a century, and the main state of the urea-formaldehyde molding compound is powder and granule. The urea-formaldehyde molding compound is produced in 1958 for the earliest time in China, the real scale is 80 years in the last century, and the first world of world production is formed at the beginning of the century.
The granular urea-formaldehyde molding compound is produced in the last 60 years, and with the development of processing machinery, the development of a high-speed automatic press and a thermosetting plastic injection molding machine is brought to the surface, and the urea-formaldehyde molding compound is required to be granulated from powder so as to meet the requirements of automatic metering and constant volume metering of processing equipment. The italian kaimei company has at least 50 years of history of granulation, but China has individual enterprises for exploration in the 90 th century at the earliest, but the scale cannot be formed, and the breakthrough of the real technology is after 2005.
The granular urea-formaldehyde molding compound has antibacterial property, and is suitable for processing toilet seat rings and covers, and the toilet seat rings and covers serving as bathroom accessory equipment need to have antibacterial property.
Plastic antibacterial agents are generally classified into organic antibacterial agents, natural antibacterial agents and inorganic antibacterial agents.
The main variety of the organic antibacterial agent is vanillin or ethyl vanillin compounds, which are commonly used in polyethylene food packaging films and play an antibacterial role. The organic antibacterial agent has the characteristics of quick response and strong sterilization capability, but is easy to generate microbial drug resistance and has the defects of easy decomposition, poor heat resistance, secondary pollution possibly caused by decomposition products and the like, so that the further application of the organic antibacterial agent is limited.
The natural antibacterial agent is mainly extracted from natural plants, such as chitin, mustard, castor oil, horseradish and the like, has the characteristics of low toxicity, high safety and simple and convenient use, but has limited antibacterial action, poor heat resistance, short service life, low sterilization rate, no broad-spectrum long-acting use and small quantity, so the use range is limited.
Plastic antimicrobials added to plastics need to meet not only low cost requirements, but also excellent compatibility and maintain high thermal stability during processing. In addition, the antimicrobial agent must also be able to migrate to the surface of the plastic, preventing microbial growth.
The inorganic antibacterial agent utilizes the antibacterial capacity of metals such as silver, copper, zinc and the like, and the metals (or ions thereof) such as silver, copper, zinc and the like are fixed on the surface of porous materials such as zeolite, silica gel and the like by methods such as physical adsorption ion exchange and the like to prepare the antibacterial agent, and then the antibacterial agent is added into corresponding products to obtain the material with the antibacterial capacity. The development and application of inorganic antibacterial agents begin in the 60's of the 20 th century, and although the inorganic antibacterial agents have relatively slow effects, the inorganic antibacterial agents have long-acting, broad-spectrum antibacterial and good chemical stability, are not easy to induce bacterial drug resistance, are safer, and particularly have outstanding heat resistance (more than 600 ℃) and have obvious industrial advantages in the application of various antibacterial agent products. The existing inorganic antibacterial agents with mature technology and wide application mainly comprise: inorganic silver-based antibacterial agents, photocatalytic antibacterial agents, zinc oxide whisker (ZnOw) composite antibacterial agents, other inorganic nano antibacterial agents and the like.
Inorganic silver-based antibacterial agent: the antibacterial agent is formed by fixing silver ions with antibacterial activity on carriers such as zirconium phosphate, silicon dioxide and the like by physical adsorption, ion exchange and the like, and the antibacterial agent slowly releases the silver ions in the using process to destroy the activity of cell membranes or protoenzyme of bacteria, thereby having the antibacterial effect. The silver-carrying inorganic antibacterial agent has the advantages of wide antibacterial spectrum, lasting antibacterial effect, difficult generation of drug resistance, good biological safety and the like. However, there are some problems that firstly, silver ions dissociated from the materials are easily reduced to simple substance silver to be gray or brown under the irradiation of sunlight or after being heated to a certain temperature, so that the color of the product is influenced; secondly, the silver raw material is precious and rare, and the cost of the silver antibacterial agent is high; in addition, it is inferior in antifungal and antifungal effects, which have hindered the use of silver-based antibacterial agents to some extent.
Photocatalytic antibacterial agents: n-type semiconductor oxides, e.g. TiO, mostly of wide bandgap2、ZnO、CdS、Fe2O3、ZnS、SiO2And the like. Wherein the anatase type TiO2Is the most common photocatalytic antibacterial agent at present. The photocatalytic antibacterial agent has a high purification effect on bacteria, fungi, mold, smelly organic matters and the like, but the material has the greatest limitation that the material has a strong antibacterial effect only under the illumination condition, and is not suitable for the material to play a role in a relatively dark environment, for example, the antibacterial plastic of sanitary bath equipment accessories in a windowless toilet has a poor effect.
Chinese patent document (publication No. CN 108819001B) discloses a manufacturing process of urea-formaldehyde molding compound particles with antibacterial, antistatic and high gloss, which needs to modify products step by melamine resin, dimethyl terephthalate, a silver ion antibacterial agent and octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate solution under a set condition according to the proportion in three procedures of kneading, ball milling and wet granulation respectively, and prepare the urea-formaldehyde molding compound particles by step modification, wherein the antibacterial agent is a silver ion water antibacterial agent with the silver content of 1000 ppm. The method has high cost and poor antifungal and antifungal effects.
The wood pulp used in urea-formaldehyde molding compound is needle pulp or broad leaf pulp, and is prepared by cooking wood slices in alkali liquor, removing lignin, rinsing with clear water, bleaching with hydrogen peroxide and drying to obtain wood pulp (roll pulp or board pulp), and applying to amino molding compound. Due to the fact that wood pulp is made of wood fibers, and the wood fibers are characterized by having capillary pores, part of resin is soaked into the capillary pores in the processing process, so that the pulp with the water content of below 30% is loose instead of being agglomerated into large lumps after kneading is finished, the surface is not very viscous, the smooth penetration of hot wind energy in the drying process is facilitated, the drying strength is favorably improved, the molding compound is prevented from being stuck to a mesh belt or being mutually bonded, and the amino coloring diversity is provided while the good processing characteristics are kept.
In the prior art, under the condition of normal pressure dehydration, wood pulp adopted by kneading in a kneader is board pulp, namely, raw sheet pulp with the size of 1200 multiplied by 1000mm is manually put into the kneader and is kneaded and dehydrated under the condition of air exhaust of an induced draft fan. The defects of the method are that the mass is more after kneading and dehydration, the diameter of the mass is large, more coarse powder is generated after ball milling, and the subsequent drying efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problem of providing a granular urea formaldehyde molding compound which is added with four-needle-shaped zinc oxide whiskers so as to enable the material to have an excellent antibacterial effect.
The invention provides a technical scheme for solving the technical problems, which comprises the following steps: the broad-spectrum lasting antibacterial granular urea formaldehyde molding compound comprises the following components in parts by weight: urea-formaldehyde resin 3120-4040 portions, four needle-like zinc oxide whisker 18-45 portions and hexamethylene tetramine 80-120 portions.
Furthermore, the tetrapod-like zinc oxide whisker is modified by a silane coupling agent, and is provided with a central body and four needle-like crystals, wherein the four needle-like bodies are all unfolded from the center of gravity of a tetrahedron to the three-dimensional direction, and the included angle between any two needles is 109 degrees.
Furthermore, the length of the needle body of the tetrapod-like zinc oxide whisker is less than or equal to 30 mu m, the diameter of the needle root body is 0.5-2 mu m, the minimum inhibitory concentration MIC is less than or equal to 200ppm, and the thermal expansion coefficient is 4.0 multiplied by 10-6percent/DEG C, heat resistance is more than or equal to 500 ℃.
Further, the broad-spectrum durable antibacterial granular urea formaldehyde molding compound also comprises the following components in parts by weight: 20-30 parts of curing agent, 30-90 parts of inorganic filler, 540-648 parts of wood pulp, 15-20 parts of lubricant, 16-20 parts of titanium dioxide, 1.5-2.2 parts of coloring pigment and 0-30 parts of polyvinyl alcohol; the urea-formaldehyde resin is prepared by reacting 1000-1200 parts of urea, 2000-2600 parts of formaldehyde, 40-120 parts of melamine and 80-120 parts of hexamethylenetetramine.
Further, the curing agent is salt generated by neutralization reaction of ethanolamine and sulfamic acid, the curing agent is colorless and transparent liquid in appearance, the solid content is 38-40 wt%, and the pH value of the solution is 7.2-7.5;
the inorganic filler is one or more of talcum powder, calcium carbonate and precipitated barium sulfate, and the fineness of the inorganic filler is 700-900 meshes;
the wood pulp is conifer reeled pulp or conifer board pulp, the whiteness is 90-92 ℃, and the PH value is 6.5-7.0;
the lubricant is one or more of stearic acid, zinc stearate and ethylene stearic acid amide;
the titanium dioxide is rutile type titanium dioxide;
the coloring pigment is an organic pigment.
Tetrapod-like zinc oxide whiskers (T-ZnOw for short) were discovered in the 40 th century and were first successfully developed in 1989 by the Japan Sonchi Kogyo industry. The appearance of the tetrapod-like zinc oxide whisker is white loose powder, and the tetrapod-like zinc oxide whisker is microscopically in a three-dimensional tetrapod-like three-dimensional structure, namely the whisker is provided with a core, four acicular crystals are stretched out from the radial direction of the core, each acicular body is a monocrystal microfiber, and the included angle of any two acicular bodies is 109 degrees. The diameter of the central body of the whisker is 0.7-1.4 mu m, the diameter of the root of the needle-shaped body is 0.5-14 mu m, the length of the needle-shaped body is 3-200 mu m, and an electron diffraction image shows that the whisker has single crystallinity with small dislocation and few lattice defects; atomic absorption spectroscopy showed that the whisker was low in impurity content and zinc oxide content was 99.95%, so that the tetrapod-like zinc oxide whisker was similar to a single crystal, which was the only whisker having a spatial three-dimensional structure among all whiskers up to now.
A whisker refers to a fiber that is naturally formed or grown in the form of a single crystal under artificially controlled conditions (main form), has a very small diameter (on the order of nanometers), does not contain defects (grain boundaries, dislocations, holes, etc.) that are usually present in materials, and has a highly ordered atomic arrangement, so that its strength is close to the theoretical value of a complete crystal. Its mechanical strength is equal to the adjacent interatomic force. The highly oriented structure of the whisker not only enables the whisker to have high strength, high modulus and high elongation, but also has the properties of electricity, light, magnetism, dielectric, electric conduction and super electric conduction. The tetrapod-like zinc oxide whisker has excellent performances which are incomparable with common zinc oxide, such as wear resistance, reinforcement, vibration reduction, skid resistance, noise reduction, aging resistance, static resistance, bacteria resistance and the like.
The antibacterial principle of the tetrapod-like zinc oxide whisker antibacterial agent is as follows:
(1)Zn+2and (3) active antibiosis: zn+2The antibacterial mechanism of (2) is similar to that of silver ions;
(2) the zinc oxide whisker tip nanometer activity is antibiotic: the tip of ZnO has a considerable part in the nanometer level, thereby having special surface effect and high activity of the nanometer material. The nanometer active components can kill and eliminate bacteria and their remains effectively and decompose toxin secreted by bacteria. In addition, four needle tip parts with nanometer effect of the tetrapod-like zinc oxide whisker can not generate agglomeration, so that the tetrapod-like zinc oxide whisker dispersible nanometer material has a true meaning and is more favorable for the exertion of antibacterial activity.
Tetrapod-like zinc oxide crystal having semiconductor characteristicsThe nano active component of the whisker tip can generate free electrons (e) in a system in which moisture and air exist-) While leaving positively charged holes (n)+) And the following reactions are gradually generated:
ZnO+nV→e-+n+
e-+O2→O2 -
n++H2O→OH+H+
generated positively charged holes (n)+) Has strong oxidation effect, hydroxyl free radical and superoxide anion free radical (O)2 -) Can destroy the thallus structure and eliminate toxin secreted by bacteria, which is a unique advantage of the tetrapod-like zinc oxide whisker.
(3) The four-needle zinc oxide whisker atomic oxygen is antibacterial: the tetrapod-like zinc oxide whisker is a semiconductor acicular fiber with adjustable internal carriers, and atomic oxygen in the crystal lattice of the semiconductor acicular fiber can destroy the bioactivity and metabolic propagation function of most bacteria.
The tetrapod-like zinc oxide whisker adopted in the invention needs surface modification because of the unique tetrapod-like structure of the tetrapod-like zinc oxide whisker, and the diameter of the tip of a needle body reaches the nanometer level. When the addition amount is less than 5 percent, the nano-crystalline silicon material is uniformly dispersed in the resin, and when the addition amount is 5 percent, the whiskers are mutually linked to form a network structure, so that the nano-crystalline silicon material is not easy to agglomerate in a particle shape or a rod shape like other nano-crystalline materials, and can be uniformly distributed in the polymer through surface modification treatment.
The invention provides another technical scheme for solving the technical problems, which comprises the following steps: a method for preparing the broad-spectrum durable antibacterial granular urea formaldehyde molding compound as claimed in claim 1, comprising the steps of:
s1: surface modification: and adding a silane coupling agent to modify the tetrapod-like zinc oxide whiskers, wherein the adding amount of the silane coupling agent is 1-2 wt% of the tetrapod-like zinc oxide whiskers, and thus obtaining the surface-modified tetrapod-like zinc oxide whiskers.
S2: resin prepolymerization: reacting formaldehyde, hexamethylenetetramine, urea and melamine to obtain a urea-formaldehyde resin prepolymer;
s3: dewatering and kneading: adding the urea-formaldehyde resin prepolymer into a vacuum kneader, adding a part of wood pulp, surface-modified tetrapod-like zinc oxide whiskers, a curing agent, an inorganic filler, a lubricant, titanium dioxide and a coloring pigment, kneading for a period of time, continuously adding the rest wood pulp, and performing vacuum kneading dehydration under the heating of jacket steam;
s4, drying: and (3) conveying the material obtained in the last step into a dryer for drying to obtain dried particles with the water content of less than 3.2%. 7. The method for preparing the broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 6, characterized by further comprising the steps of:
s5, crushing, ball milling and powder sieving: crushing, ball-milling and sieving the dried particles in sequence to obtain fine powder with certain fineness;
s6, granulating and drying: adding a binder into the fine powder in a granulator for granulation, and then drying to obtain dry granules;
s7, straightening and mixing: and (4) granulating the dried granules in a granulator, separating by using a vibrating screen, and mixing the granules with the fineness of 14-60 meshes in a mixer to obtain a finished product.
Further, in the step S1, adding metered tetrapod-like zinc oxide whiskers into a high-speed stirrer, spraying a diluted silane coupling agent, wherein the added weight of the silane coupling agent is 1% -2% of that of the tetrapod-like zinc oxide whiskers, stirring at a high speed for 30 minutes, heating an outer jacket of the high-speed stirrer by using steam, and controlling the pressure intensity to be 0.1-0.15 MPa, then performing vacuum-pumping drying for 25-35 min under a low-speed operation condition, releasing the vacuum, releasing the jacket steam, and then cooling at a low speed for 50-70 min to obtain surface-modified tetrapod-like zinc oxide whiskers;
step S2, adding the metered formaldehyde into a reaction kettle, and starting a stirring paddle of the reaction kettle, wherein the rotating speed of the stirring paddle of the reaction kettle is 50-80 rpm; then adding metered hexamethylene tetramine, and adding metered urea after the hexamethylene tetramine is completely dissolved and the pH value of the solution is measured to be 7.0-7.5 by sampling; when the urea is dissolved and the temperature of the material is not reduced any more, opening a steam valve to supply air, controlling the pressure at 0.08-0.085 MPa, and heating the material by a jacket; when the temperature of the material rises to 25-35 ℃, closing steam, and generating hydroxymethyl urea and dimethylol urea by the material due to addition reaction to release heat; adding metered melamine when the temperature is automatically raised to about 50 ℃, starting prepolymerization, and finishing prepolymerization when the temperature is raised to 60 ℃ to obtain prepolymerized urea-formaldehyde resin;
step S3, pre-polymerized urea-formaldehyde resin is put into a vacuum kneader, and half of the cut and metered wood pulp, surface modified tetrapod-like zinc oxide whiskers, and metered curing agent, inorganic filler, lubricant, titanium dioxide and coloring pigment are added; starting the blades of the vacuum kneader, kneading the blades of the vacuum kneader for 8-10 min at the rotating speed of 22-40 rpm, adjusting the blades to operate in the opposite direction, and continuously adding the other half of the metered wood pulp; then starting steam to heat the kneading machine, and controlling the steam pressure to be 0.095 MPa-0.098 MPa; starting a vacuum pump to perform air suction and dehydration, gradually increasing the vacuum degree from 0.08MPa to 0.095MPa from 0.08MPa, performing dehydration for 50-55 min, closing steam when the materials are observed to be loose and small particles, continuously cooling for 4-6 min, then relieving the vacuum, opening a bottom valve to discharge materials, and finishing dehydration and kneading;
step S4, after the dehydration kneading is finished, the material is continuously and uniformly paved on a drying belt by a material distributor and enters a dryer, the thickness of the material layer of the material entering the dryer on the drying belt is 7 cm-8 cm, the drying time in the dryer is 130-150 min, and the dried material becomes dry fine particles;
step S5, after the dry fine particles continuously enter a crusher to be crushed, the dry fine particles enter a cyclone dust removal integrated machine to be subjected to gas-solid separation; the solid particles fall into a ball mill for ball milling, the materials are milled in the ball mill for 4 to 6 hours and then conveyed into a screening machine for screening, and fine powder reaching 80 meshes enters a granulation step;
step S6, uniformly spraying a binder into the fine powder obtained in step S5 in granulation equipment, wherein the fine powder is formed into round or oval fine particles by utilizing the action of centrifugal force in the granulation equipment, the round or oval fine particles are bonded into a compact granular material by the powder under the action of the binder, the granulation time is 15-20 min, and then the granular material is input into a dryer to be dried by hot air, the air temperature is 75-80 ℃, and the drying time is 30-35 min;
and step S7, the dried material particles are arranged into a whole by a granulator, sieved by a rotary vibration sieve, and formed into semi-finished products by 14-60 meshes of fine particles, and the semi-finished products are continuously sent into a mixer for mixing for 30min, and then discharged and packaged into finished products to be stored.
Further, in the step S4, an air blower sucks outside air into the dryer, the air entering the dryer is heated to a set temperature of 80-100 ℃ by a heat exchanger, and then penetrates through the material layer on the drying belt to dry the material; and one part of air penetrating through the material layer on the drying belt is sucked into the dryer by the air feeder for recycling, and the other part of air is pumped out by the induced draft fan and enters the scrubbing tower for absorbing residual formaldehyde for purification treatment.
Further, the granulation in the step S6 is a wet granulation process, in which a binder is uniformly sprayed into the fine powder obtained in the step S5 in a granulator, the fine powder is made into round or oval granules by the action of centrifugal force in the granulator, the granules are bound from the powder into granules by the action of the binder, the mass of each batch is 95 to 105kg, and the granulation time is 15 to 25 min;
still further, the preparation method of the binder in the step S6 is: adding water into 20-30 parts of metered polyvinyl alcohol to dissolve and dilute the polyvinyl alcohol into 1-2% aqueous solution to prepare a binder;
still further, the preparation method of the binder in the step S6 is: taking out 1% -2% of urea-formaldehyde resin obtained by prepolymerization in the step S2, and adding water for dilution, wherein the weight ratio of the urea-formaldehyde resin to the water is 1: 9, preparing the adhesive.
The invention has the following positive effects:
(1) the granular urea formaldehyde molding compound with the broad-spectrum lasting antibacterial property is added with the tetrapod-like zinc oxide whiskers, the tetrapod-like zinc oxide whiskers are the only whiskers with the spatial three-dimensional structure so far, the defect that a common silver inorganic antibacterial agent is easy to discolor is overcome, the granular urea formaldehyde molding compound with the broad-spectrum lasting antibacterial property can be used for resisting bacteria by means of ultraviolet light catalysis unlike a photocatalytic antibacterial material, secondary pollution and other side effects cannot be caused like an organic antibacterial agent, and the granular urea formaldehyde molding compound is an all-weather inorganic antibacterial agent. The broad-spectrum lasting antibacterial granular urea formaldehyde molding compound is mainly used as a forming processing material of low-voltage electric appliances such as matching parts of high-grade sanitary wares, electrical switches, electric appliance shells, sockets, circuit breakers and the like and lighting appliances, and has excellent antibacterial effect in the application period of products under dry and wet conditions.
(2) The strength and modulus of the tetrapod-like zinc oxide whiskers of the broad-spectrum durable antibacterial granular urea-formaldehyde molding compound are close to the theoretical strength of the valence bonds between atoms of the material due to the highly ordered atomic arrangement structure, and the tetrapod-like zinc oxide whiskers are isotropic, so that the tetrapod-like zinc oxide whiskers have a strong toughening effect on the composite material.
(3) The broad-spectrum lasting antibacterial granular urea-formaldehyde molding compound overcomes the defects of various antibacterial agents in the existing granular urea-formaldehyde molding compound for the toilet seat cover, and zinc oxide whiskers are used as the antibacterial agent, so that the zinc oxide whiskers can be well dispersed in a urea-formaldehyde molding compound system, the molding compound is endowed with broad-spectrum, high-efficiency and lasting antibacterial property, and the effects of antistatic property, wear resistance, skid resistance, fragmentation resistance and isotropy enhancement are improved. The antibacterial activity of the tetrapod-like zinc oxide whiskers is stronger and longer than that of the traditional antibacterial agent.
(4) The preparation method of the broad-spectrum durable antibacterial granular urea-formaldehyde molding compound puts the surface-modified tetrapod-like zinc oxide whiskers used as the antibacterial agent into the vacuum kneader together with other auxiliary materials in the dehydration kneading in the step S3, which is beneficial to enhancing and lasting antibacterial activity of the prepared granular urea-formaldehyde molding compound and has better mechanical property and antibacterial effect.
(5) The preparation method of the broad-spectrum lasting antibacterial granular urea formaldehyde molding compound has the advantages that vacuum kneading dehydration is performed after wood pulp is chopped, so that the effect is more uniform, the agglomeration is reduced, the diameter of the agglomeration is smaller, the generation of coarse powder after ball milling is reduced, the drying efficiency of a dryer is improved, and more urea formaldehyde molding compounds are obtained.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a broad-spectrum durable antibacterial granular urea formaldehyde molding compound of the present invention.
Detailed description of the invention
Example 1
The broad-spectrum lasting antibacterial granular urea formaldehyde molding compound comprises the following components in parts by weight: 1200 parts of urea, 2000 parts of formaldehyde, 120 parts of melamine, 22 parts of tetrapod-like zinc oxide whiskers, 120 parts of hexamethylenetetramine, 20 parts of a curing agent, 90 parts of talcum powder, 540 parts of conifer pulp, 15 parts of stearic acid, 20 parts of rutile titanium dioxide and 2.2 parts of organic yellow.
Referring to fig. 1, the preparation method of the broad-spectrum durable antibacterial granular urea formaldehyde molding compound of this embodiment 1 includes the following steps:
s1: surface modification: the surface modification of the tetrapod-like zinc oxide whisker by activating treatment is carried out by a silane coupling agent, the surface modification of the activating treatment is carried out in a high-speed stirrer, and the method comprises the following steps: adding tetrapod-like zinc oxide whiskers into a high-speed stirrer, spraying a diluted silane coupling agent, wherein the weight of the diluted silane coupling agent is 1% -2% of that of the tetrapod-like zinc oxide whiskers, stirring at a high speed for 30 minutes, heating an outer jacket of the high-speed stirrer by using steam, and controlling the pressure to be 0.1-0.15 MPa, then vacuumizing and drying for 30 minutes under the condition of low-speed operation, releasing vacuum, releasing jacket steam, and cooling at a low speed for a while to obtain the surface-modified tetrapod-like zinc oxide whiskers.
S2: pre-polymerization of urea resin: putting the measured formaldehyde into a reaction kettle, and starting a stirring paddle of the reaction kettle, wherein the rotating speed of the stirring paddle of the reaction kettle is 50-80 rpm; slowly adding metered hexamethylene tetramine, and adding metered urea after the hexamethylene tetramine is completely dissolved and sampled to obtain a solution with a pH value of 7.0-7.5 (precision test paper); the material temperature is obviously reduced along with the change of the dissolved solution of the urea from milky white to clear; when the urea is dissolved and the temperature of the material is not reduced any more, opening a steam valve to supply air, controlling the pressure at 0.08-0.085 MPa, and heating the material by a jacket; when the temperature of the material rises to 25-35 ℃, the steam is closed, and the material generates heat due to the addition reaction to generate hydroxymethyl urea and dimethylol urea; and (3) adding metered melamine when the temperature is automatically raised to about 50 ℃, starting prepolymerization, and finishing prepolymerization when the temperature is raised to 60 ℃ to obtain prepolymerized urea-formaldehyde resin, wherein the whole prepolymerization time is 60 min.
The urea resin obtained by the prepolymerization is subjected to a S2 dehydration kneading step.
S3: dewatering and kneading: putting the pre-polymerized urea-formaldehyde resin into a vacuum kneader, and adding the cut and metered half of wood pulp, the surface-modified tetrapod-like zinc oxide whiskers and the metered curing agent, the inorganic filler, the lubricant, the titanium dioxide and the coloring pigment; starting the paddle of the vacuum kneader, kneading the paddle shaft of the vacuum kneader at the rotating speed of 40rpm for 8min, adjusting the paddle to run in the opposite direction, and continuously adding the other half of the metered wood pulp; then starting steam to heat the kneading machine, and controlling the steam pressure to be 0.095 MPa-0.098 MPa; and starting a vacuum pump to perform air suction and dehydration, wherein the vacuum degree is increased along with the reduction of the moisture content and gradually increased from 0.08MPa to 0.095MPa, the dehydration time is 50min, when the material becomes loose small particles, closing steam and continuously cooling for 4min, then releasing the vacuum, opening a bottom valve to discharge the material, inputting the material into a first buffer through a conveyor belt, and finishing dehydration and kneading.
The material entering the first buffer is loose particles with water content of 26% +/-2%.
S4: and (3) drying: after the dehydration kneading is finished, the material entering the buffer I is conveyed by a conveying belt to enter a distributing device, the material is continuously and uniformly laid on a drying belt by the distributing device to enter a dryer, the thickness of the material layer of the material entering the dryer on the drying belt is 7 cm-8 cm, the drying time in the dryer is 130min, and the dried material becomes dry fine particles with the water content of 3% +/-0.2%.
S41: sucking outside air into the dryer in the step S4 by a blower, heating the air entering the dryer to a set temperature of 80-100 ℃ by a heat exchanger, and penetrating through a material layer on a drying belt to dry the material; and one part of air penetrating through the material layer on the drying belt is sucked into the dryer by the air feeder for recycling, and the other part of air is pumped out by the induced draft fan and enters the scrubbing tower for absorbing residual formaldehyde for purification treatment.
S5: crushing and ball-milling: the dried fine particles are lifted to a conveyer belt by a packing auger at the tail part of the dryer, continuously enter a crusher for crushing, and then enter a cyclone dust removal integrated machine for gas-solid separation by air conveying through a pipeline; the solid particles fall into a ball mill for ball milling, and residual gas is dedusted by a cloth bag and then discharged into a gas washing tower by a vacuum pump for purification treatment; after the fine materials are ground in the ball mill for 4-6 h, the fine materials are conveyed into a screening machine for screening by a second buffer and a discharge auger in a rated mode, fine powder reaching 80 meshes enters a granulation step, and coarse powder is intensively returned to the ball mill for ball milling processing again.
S6: granulating and drying: dissolving and diluting polyvinyl alcohol into 1% aqueous solution as a binder; and (3) uniformly spraying a binder into the fine powder obtained in the step (S5) in a granulating device, wherein the fine powder is formed into round or oval fine particles by the action of centrifugal force in the granulating device, the fine powder is bonded into a compact granular material by the action of the binder, the granulating time is 15min, and then the granular material is conveyed into a flat plate dryer to be dried by hot air, the air temperature is 75-80 ℃, and the drying time is 30 min. At this time, the granulated material was dried granules having a water content of 3% + -0.2%.
S7: finishing, screening and mixed packaging: feeding the dry material particles into an elevated tank by wind, then arranging the dry material particles by a granulator through the elevated tank, screening the dry material particles by a rotary vibration sieve, forming semi-finished products from 14-60 meshes of fine particles, continuously feeding the semi-finished products into a mixer for mixing for 30min, and then discharging and packaging the semi-finished products into finished products to be put in storage; returning the coarse powder to the ball mill for ball milling, and repeating the steps from S5 to S7; returning the fine powder to the granulating equipment for granulating and drying, and repeating the steps from S6 to S7.
Example 2
The broad-spectrum lasting antibacterial granular urea formaldehyde molding compound comprises the following components in parts by weight: 1150 parts of urea, 2400 parts of formaldehyde, 80 parts of melamine, 33 parts of tetrapod-like zinc oxide whiskers, 100 parts of hexamethylenetetramine, 28 parts of a curing agent, 60 parts of calcium carbonate, 600 parts of conifer board pulp, 15 parts of zinc stearate, 20 parts of rutile titanium dioxide and 2 parts of high-pigment carbon black.
The preparation method of the broad-spectrum lasting antibacterial granular urea formaldehyde molding compound of the embodiment 2 comprises the following steps:
s1: surface modification: the surface modification of the tetrapod-like zinc oxide whisker by activating treatment is carried out by a silane coupling agent, the surface modification of the activating treatment is carried out in a high-speed stirrer, and the method comprises the following steps: firstly adding tetrapod-like zinc oxide whiskers into a high-speed stirrer, spraying a diluted silane coupling agent, wherein the weight of the diluted silane coupling agent accounts for 1-2% of that of the tetrapod-like zinc oxide whiskers, stirring at a high speed for 30 minutes, heating an outer jacket of the high-speed stirrer by using steam, and controlling the pressure to be 0.1-0.15 MPa, then vacuumizing and drying for 30 minutes under the condition of low-speed operation, relieving the vacuum, relieving the steam of the jacket, and cooling for a while at a low speed to obtain the surface-modified tetrapod-like zinc oxide whiskers.
S2: pre-polymerization of urea resin: putting the measured formaldehyde into a reaction kettle, and starting a stirring paddle of the reaction kettle, wherein the rotating speed of the stirring paddle of the reaction kettle is 50-80 rpm; slowly adding metered hexamethylene tetramine, and adding metered urea after the hexamethylene tetramine is completely dissolved and sampled to obtain a solution with a pH value of 7.0-7.5 (precision test paper); the material temperature is obviously reduced along with the change of the dissolved solution of the urea from milky white to clear; when the urea is dissolved and the temperature of the material is not reduced any more, opening a steam valve to supply air, controlling the pressure at 0.08-0.085 MPa, and heating the material by a jacket; when the temperature of the material rises to 25-35 ℃, closing steam, and generating hydroxymethyl urea and dimethylol urea by the material due to addition reaction to release heat; and (3) adding metered melamine when the temperature is automatically raised to about 50 ℃, starting prepolymerization, and finishing prepolymerization when the temperature is raised to 60 ℃ to obtain prepolymerized urea-formaldehyde resin, wherein the whole prepolymerization time is 60 min.
Taking out 1-2% of the urea-formaldehyde resin obtained by prepolymerization in the step for later use, and performing dehydration and kneading on the rest in S2.
S3: dewatering and kneading: putting the pre-polymerized urea-formaldehyde resin into a vacuum kneader, and adding the cut and metered half of wood pulp, the surface-modified tetrapod-like zinc oxide whiskers and the metered curing agent, the inorganic filler, the lubricant, the titanium dioxide and the coloring pigment; starting the paddle of the vacuum kneader, kneading the paddle shaft of the vacuum kneader at the rotating speed of 40rpm for 8min, adjusting the paddle to run in the opposite direction, and continuously adding the other half of the metered wood pulp; then starting steam to heat the kneading machine, and controlling the steam pressure to be 0.095 MPa-0.098 MPa; and starting a vacuum pump to perform air suction and dehydration, wherein the vacuum degree is increased along with the reduction of the moisture content and gradually increased from 0.08MPa to 0.095MPa, the dehydration time is 50min, when the material becomes loose small particles, closing steam and continuously cooling for 4min, then releasing the vacuum, opening a bottom valve to discharge the material, inputting the material into a first buffer through a conveyor belt, and finishing dehydration and kneading.
The material entering the first buffer is loose particles with water content of 26% +/-2%.
S4: and (3) drying: after the dehydration kneading is finished, the material entering the buffer I is conveyed by a conveying belt to enter a distributing device, the material is continuously and uniformly laid on a drying belt by the distributing device to enter a dryer, the thickness of the material layer of the material entering the dryer on the drying belt is 7 cm-8 cm, the drying time in the dryer is 130min, and the dried material becomes dry fine particles with the water content of 3% +/-0.2%.
S41: sucking outside air into the dryer in the step S4 by a blower, heating the air entering the dryer to a set temperature of 80-100 ℃ by a heat exchanger, and penetrating through a material layer on a drying belt to dry the material; and one part of air penetrating through the material layer on the drying belt is sucked into the dryer by the air feeder for recycling, and the other part of air is pumped out by the induced draft fan and enters the scrubbing tower for absorbing residual formaldehyde for purification treatment.
S5: crushing and ball-milling: the dried fine particles are lifted to a conveyer belt by a packing auger at the tail part of the dryer, continuously enter a crusher for crushing, and then enter a cyclone dust removal integrated machine for gas-solid separation by air conveying through a pipeline; the solid particles fall into a ball mill for ball milling, and residual gas is dedusted by a cloth bag and then discharged into a gas washing tower by a vacuum pump for purification treatment; after the fine materials are ground for 4h6 in the ball mill, the fine materials are conveyed into a screening machine for screening by a buffer II and a discharge auger in a rated mode, fine powder reaching 80 meshes enters a granulation step, and coarse powder is intensively returned to the ball mill for ball milling processing again.
S6: granulating and drying: diluting the urea-formaldehyde resin obtained by prepolymerization with water, wherein the weight ratio of the urea-formaldehyde resin to the water is 1: 9, using the prepared aqueous solution as a binder; and (3) uniformly spraying a binder into the fine powder obtained in the step (S5) in a granulating device, wherein the fine powder is formed into round or oval fine particles by the action of centrifugal force in the granulating device, the fine powder is bonded into a compact granular material by the action of the binder, the granulating time is 15min, and then the granular material is conveyed into a flat plate dryer to be dried by hot air, the air temperature is 75-80 ℃, and the drying time is 30 min. At this time, the granulated material was dried granules having a water content of 3% + -0.2%.
S7: granulating, screening, mixing and packaging: feeding the dry material particles into an elevated tank by wind, then arranging the dry material particles by a granulator through the elevated tank, screening the dry material particles by a rotary vibration sieve, forming semi-finished products from 14-60 meshes of fine particles, continuously feeding the semi-finished products into a mixer for mixing for 30min, and then discharging and packaging the semi-finished products into finished products to be put in storage; returning the coarse powder to the ball mill for ball milling, and repeating the steps from S5 to S7; and returning the fine powder to a granulating device for granulating and drying, and repeating the steps from S6 to S7.
Example 3
The broad-spectrum lasting antibacterial granular urea formaldehyde molding compound comprises the following components in parts by weight: 1000 parts of urea, 2600 parts of formaldehyde, 40 parts of melamine, 44 parts of tetrapod-like zinc oxide whiskers, 80 parts of hexamethylenetetramine, 30 parts of a curing agent, 30 parts of precipitated barium sulfate, 640 parts of conifer rolling stock, 19 parts of ethylene stearamide, 16 parts of rutile titanium dioxide and 2 parts of organic blue.
The preparation method of the broad-spectrum durable antibacterial granular urea formaldehyde molding compound of the embodiment 3 is the same as that of the embodiment 2, except that the parts of the raw materials are different.
The raw material formulation components of examples 1 to 3 of the present invention are shown in table 1 in parts by weight.
Table 1 raw material formula composition table
The invention takes AT-831 type tetrapod-like zinc oxide crystal whisker provided by southwest intersection Dajingyu science and technology Limited company as an antibacterial agent after surface modification. The properties of AT-831 type tetrapod-like zinc oxide whiskers are shown in Table 2.
TABLE 2 Performance Table of AT-831 type tetrapod-like zinc oxide whisker
| Item | Index (I) |
| Appearance of the product | White or near-white powder |
| Needle length (mum) | ≤30 |
| Root diameter of needle-like body (mum) | 0.5～2 |
| Minimum inhibitory concentration MIC (PPM) | ≤200 |
| Oral toxicity LD50(mg/kg) | Greater than or equal to 10000 (actually non-toxic) |
| Irritation property | Has no irritation to eyes and skin |
| Coefficient of thermal expansion (%/deg.C) | 4.1×10-6 |
| Heat resistance (. degree. C.) | ≥500 |
The curing agent is a salt (SE for short) generated by neutralization reaction of ethanolamine and sulfamic acid, the appearance of the curing agent is colorless and transparent liquid, the solid content is 38-40%, and the pH value of the solution is 7.2-7.5. The fineness of the inorganic filler is 700-900 meshes. The wood pulp is conifer rolling pulp or conifer board pulp produced by GP company, the whiteness is 90-92 ℃, the PH value is 6.5-7.0, and the wood pulp is cut into small blocks with the size not larger than 20 multiplied by 20 mm. Rutile titanium dioxide was DuPont 902. The coloring pigment is a Ciba-Jia-based organic pigment.
The broad-spectrum durable antibacterial granular urea-formaldehyde molding compound prepared in the examples 1 to 3 and a normal urea-formaldehyde molding compound (comparative example) using silver ion water as an antibacterial agent are subjected to a comparative test, samples prepared and subjected to performance measurement according to GB/T13454-92 are subjected to sample pressing, and samples of the appendix A molding shrinkage, GB9341 bending strength, GB1043 impact strength and notch impact strength standard of the simply supported beam are subjected to actual test, and the data are summarized as shown in Table 3.
TABLE 3 granular urea-formaldehyde molding compound parameter table
The granular urea-formaldehyde molding materials having a long-lasting broad-spectrum antibacterial property obtained in examples 1 to 3 and the urea-formaldehyde molding materials (comparative examples) having silver ion water as an antibacterial agent were processed into toilet seat covers, respectively, and then the antibacterial effects were measured, as shown in Table 4.
TABLE 4 antibacterial effect of antibacterial granular urea-formaldehyde molding compound product
After the broad-spectrum lasting antibacterial granular urea-formaldehyde molding compound prepared in examples 1 to 3 and a normal urea-formaldehyde molding compound (comparative example) using silver ion water as an antibacterial agent are respectively processed into a toilet seat cover, a cold and hot fatigue test method of 6.21 in building material industry standard JC/T764-2008 of toilet seat and cover (the toilet seat and cover are respectively placed in a container at 70 ℃ plus or minus 3 ℃ and a refrigerator at-20 ℃ plus or minus 3 ℃ for 3 hours, and are dried for 24 hours at the ambient temperature of 22 ℃ plus or minus 3 ℃ after 5 cycles), the urea-formaldehyde molding compound is subjected to an accelerated aging test, and then the antibacterial durability of the urea-formaldehyde molding compound is observed, and the obtained data are shown in Table 5.
TABLE 5 antibacterial effect of the antibacterial granular urea formaldehyde molding compound after aging
The test results show that the surface-modified AT-831 type tetrapod-like zinc oxide whiskers added into the broad-spectrum durable antibacterial granular urea-formaldehyde molding compound are better in mechanical property and antibacterial effect compared with the urea-formaldehyde molding compound added with silver ion water as an antibacterial agent, and particularly, the antibacterial rate of a processed product of the urea-formaldehyde molding compound is better than that of a urea-formaldehyde molding compound product added with silver ion water as an antibacterial agent after a cold and hot fatigue test.
Claims (10)
1. The broad-spectrum lasting antibacterial granular urea formaldehyde molding compound is characterized by comprising the following components in parts by weight: urea-formaldehyde resin 3120-4040 portions and tetrapod-like zinc oxide whisker 18-45 portions.
2. The broad-spectrum durable antibacterial granular urea formaldehyde molding compound as claimed in claim 1, characterized in that: the four-needle-shaped zinc oxide whisker is modified by a silane coupling agent and is provided with a central body and four needle-shaped crystals, the four needle-shaped bodies are unfolded from the gravity center of a tetrahedron to the three-dimensional direction, and the included angle between any two needles is 109 degrees.
3. The broad-spectrum durable antibacterial granular urea formaldehyde molding compound as claimed in claim 2, characterized in that: the length of the needle body of the tetrapod-shaped zinc oxide whisker is less than or equal to 30 mu m, the diameter of the needle root body is 0.5-2 mu m, the minimum inhibitory concentration MIC is less than or equal to 200ppm, and the thermal expansion coefficient is 4.0 multiplied by 10-6percent/DEG C, heat resistance is more than or equal to 500 ℃.
4. The broad-spectrum durable antibacterial granular urea formaldehyde molding compound as claimed in claim 1, characterized in that: the paint also comprises the following components in parts by weight: 20-30 parts of curing agent, 30-90 parts of inorganic filler, 540-648 parts of wood pulp, 15-20 parts of lubricant, 16-20 parts of titanium dioxide, 1.5-2.2 parts of coloring pigment and 0-30 parts of polyvinyl alcohol; the urea-formaldehyde resin is prepared by reacting 1000-1200 parts of urea, 2000-2600 parts of formaldehyde, 40-120 parts of melamine and 80-120 parts of hexamethylenetetramine.
5. The broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 4, characterized in that: the curing agent is salt generated by neutralization reaction of ethanolamine and sulfamic acid, the appearance of the curing agent is colorless and transparent liquid, the solid content is 38-40 wt%, and the pH value of the solution is 7.2-7.5;
the inorganic filler is one or more of talcum powder, calcium carbonate and precipitated barium sulfate, and the fineness of the inorganic filler is 700-900 meshes;
the wood pulp is conifer reeled pulp or conifer board pulp, the whiteness is 90-92 ℃, and the PH value is 6.5-7.0;
the lubricant is one or more of stearic acid, zinc stearate and ethylene stearic acid amide;
the titanium dioxide is rutile type titanium dioxide;
the coloring pigment is an organic pigment.
6. The preparation method of the broad-spectrum durable antibacterial granular urea formaldehyde molding compound as claimed in claim 1, characterized by comprising the following steps:
s1: surface modification: adding a silane coupling agent to modify the tetrapod-like zinc oxide whiskers, wherein the adding amount of the silane coupling agent is 1-2 wt% of the tetrapod-like zinc oxide whiskers, and obtaining surface-modified tetrapod-like zinc oxide whiskers;
s2: resin prepolymerization: reacting formaldehyde, hexamethylenetetramine, urea and melamine to obtain a urea-formaldehyde resin prepolymer;
s3: dewatering and kneading: adding the urea-formaldehyde resin prepolymer into a vacuum kneader, adding a part of wood pulp, surface-modified tetrapod-like zinc oxide whiskers, a curing agent, an inorganic filler, a lubricant, titanium dioxide and a coloring pigment, kneading for a period of time, continuously adding the rest wood pulp, and performing vacuum kneading dehydration under the heating of jacket steam;
s4, drying: and (3) conveying the material obtained in the last step into a dryer for drying to obtain dried particles with the water content of less than 3.2%.
7. The method for preparing the broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 6, characterized by further comprising the steps of:
s5, crushing, ball milling and powder sieving: crushing, ball-milling and sieving the dried particles in sequence to obtain fine powder with certain fineness;
s6, granulating and drying: adding a binder into the fine powder in a granulator for granulation, and then drying to obtain dry granules;
s7, straightening and mixing: and (4) granulating the dried granules in a granulator, separating by using a vibrating screen, and mixing the granules with the fineness of 14-60 meshes in a mixer to obtain a finished product.
8. The method of preparing the broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 7, characterized in that: step S1, adding metered tetrapod-like zinc oxide whiskers into a high-speed stirrer, spraying a diluted silane coupling agent, wherein the adding weight of the silane coupling agent is 1% -2% of that of the tetrapod-like zinc oxide whiskers, stirring at a high speed for 30 minutes, heating an outer jacket of the high-speed stirrer by using steam, controlling the pressure intensity to be 0.1-0.15 MPa, then vacuumizing and drying for 25-35 min under the low-speed running condition, removing the vacuum, removing the steam of the jacket, and then cooling at a low speed for 50-70 min to obtain surface-modified tetrapod-like zinc oxide whiskers;
step S2, adding the metered formaldehyde into a reaction kettle, and starting a stirring paddle of the reaction kettle, wherein the rotating speed of the stirring paddle of the reaction kettle is 50-80 rpm; then adding metered hexamethylene tetramine, and adding metered urea after the hexamethylene tetramine is completely dissolved and the pH value of the solution is measured to be 7.0-7.5 by sampling; when the urea is dissolved and the temperature of the material is not reduced any more, opening a steam valve to supply air, controlling the pressure at 0.08-0.085 MPa, and heating the material by a jacket; when the temperature of the material rises to 25-35 ℃, the steam is closed, and the material generates heat due to the addition reaction to generate hydroxymethyl urea and dimethylol urea; adding metered melamine when the temperature is automatically raised to about 50 ℃, starting prepolymerization, and finishing prepolymerization when the temperature is raised to 60 ℃ to obtain prepolymerized urea-formaldehyde resin;
step S3, pre-polymerized urea-formaldehyde resin is put into a vacuum kneader, and half of the cut and metered wood pulp, surface modified tetrapod-like zinc oxide whiskers, and metered curing agent, inorganic filler, lubricant, titanium dioxide and coloring pigment are added; starting the blades of the vacuum kneader, kneading the blades of the vacuum kneader at the rotating speed of 22-40 rpm for 8-10 min, adjusting the blades to run in the opposite direction, and continuously adding the other half of the metered wood pulp; then starting steam to heat the kneading machine, and controlling the steam pressure to be 0.095 MPa-0.098 MPa; starting a vacuum pump to perform air suction and dehydration, gradually increasing the vacuum degree from 0.08MPa to 0.095MPa from 0.08MPa, performing dehydration for 50-55 min, closing steam when the materials are observed to be loose and small particles, continuously cooling for 4-6 min, then relieving the vacuum, opening a bottom valve to discharge materials, and finishing dehydration and kneading;
step S4, after the dehydration kneading is finished, the material is continuously and uniformly paved on a drying belt by a material distributor and enters a dryer, the thickness of the material layer of the material entering the dryer on the drying belt is 7 cm-8 cm, the drying time in the dryer is 130-150 min, and the dried material becomes dry fine particles;
step S5, after the dry fine particles continuously enter a crusher to be crushed, the dry fine particles enter a cyclone dust removal integrated machine to be subjected to gas-solid separation; the solid particles fall into a ball mill for ball milling, the materials are milled in the ball mill for 4 to 6 hours and then conveyed into a screening machine for screening, and fine powder reaching 80 meshes enters a granulation step;
step S6, uniformly spraying a binder into the fine powder obtained in step S5 in granulation equipment, wherein the fine powder is formed into round or oval fine particles by utilizing the action of centrifugal force in the granulation equipment, the round or oval fine particles are bonded into a compact granular material by the powder under the action of the binder, the granulation time is 15-20 min, and then the granular material is input into a dryer to be dried by hot air, the air temperature is 75-80 ℃, and the drying time is 30-35 min;
and step S7, the dried material particles are arranged into a whole by a granulator, sieved by a rotary vibration sieve, and formed into semi-finished products by 14-60 meshes of fine particles, and the semi-finished products are continuously sent into a mixer for mixing for 30min, and then discharged and packaged into finished products to be stored.
9. The method of preparing the broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 8, characterized in that: in the step S4, an air blower sucks outside air into the dryer, the air entering the dryer is heated to a set temperature of 80-100 ℃ through a heat exchanger, and then penetrates through a material layer on the drying belt to dry the material; and one part of air penetrating through the material layer on the drying belt is sucked into the dryer by the air feeder for recycling, and the other part of air is pumped out by the induced draft fan and enters the scrubbing tower for absorbing residual formaldehyde for purification treatment.
10. The preparation method of the broad-spectrum durable antibacterial granular urea formaldehyde molding compound according to claim 8, characterized by comprising the following steps: the granulation in the step S6 is a wet granulation process, in which a binder is uniformly sprayed into the fine powder obtained in the step S5 in a granulator, the fine powder is made into round or oval granules by the action of centrifugal force in the granulator, the granules are bound from the powder under the action of the binder, the mass of each batch is 95 to 105kg, and the granulation time is 15 to 25 min; the preparation method of the binder in the step S6 is: adding water into 20-30 parts of metered polyvinyl alcohol to dissolve and dilute the polyvinyl alcohol into 1-2% aqueous solution to prepare a binder; alternatively, the preparation method of the binder in step S6 is: taking out 1% -2% of urea-formaldehyde resin obtained by prepolymerization in the step S2, and adding water for dilution, wherein the weight ratio of the urea-formaldehyde resin to the water is 1: 9, preparing the adhesive.
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