CN106367020A - Anti-aging mould-proof type organic silicone sealant preparation method - Google Patents

Abstract

The invention discloses an anti-aging mould-proof type organic silicone sealant preparation method, and belongs to the technical field of organic silicone sealants. The preparation method comprises the steps of taking rotted eggs and soaking the eggs in zinc chloride solution, and enabling zinc ion and egg white to be chelated; then collecting egg white, grinding and drying the egg white, and enabling egg white chelated zinc to be hydrolyzed into polypeptide chelated zinc by enzymolysis; then using ammonium hydroxide as a precipitator to enable the polypeptide chelated zinc to be slowly released and settle, and calcining to obtain flocculent nanometer zinc oxide which is used as an anti-aging and mould-proof ingredient; utilizing a camphor tree leaf extract to further achieve a long-acting mould-proof effect; finally kneading with silicone rubber and methyl silicone oil in a vacuum mode, and filling and sealing to obtain the anti-aging mould-proof type organic silicone sealant. According to the preparation method, the zinc is in complexation with proteolytic polypeptide, the nanometer zinc oxide which is obtained after sedimentation reaction can overcome the defect that a traditional organic silicone sealant is not excellent in anti-aging property, and the corrosion resistance of the sealant can be further reinforced through preservative solution extracted from the camphor tree leaf; thus, the preparation method has wide application prospect.

Description

A kind of preparation method of ageing-resistant mould-proof-type organosilicon sealant

Technical field

The invention discloses a kind of preparation method of ageing-resistant mould-proof-type organosilicon sealant, belong to organosilicon sealant skill Art field.

Background technology

In order to adapt to the flexible and flexing causing because of the effect of extraneous factor (as temperature change), tunnel, bridge, road The concrete plates such as road, airfield runway, square are all designed with variator.Sealing variator is in concrete slab block structure Weak link, if joint seal is bad, easily allows foreign body gather in gap, hinders normally stretching of seam；In addition, also can Cause seam to seep water, soften and corrode ground, so that plate is settled or rupture, so must abutment joint be sealed.Preferably mix Solidifying soil seam joint filling encapsulant should have following performance: has lasting adhesive property, good elasticity with concrete plate With resist displacement ability, weather-resistant performance of excellent resistance to water, splendid high and low temperature resistance and brilliance etc.；Therein Durability and resistance to water directly influence serviceability and the service life of concrete slab block structure.

Room temperature organosilicon sealant due to its series of advantages such as cold-resistant, easy to use, in the every field of national economy Obtain extensive application.This kind of fluid sealant is as a kind of important bonding and encapsulant in the neck such as building and electric equipment products Domain has been widely used, and especially in the waterproof sealing of the aspects such as kitchen, washroom, Electronic Packaging product, it is even more not The material that can or lack.However, there is a typical shortcoming in room temperature organosilicon sealant, that is, if it is located after solidifying for a long time Easily grow various mycetes under hygrothermal environment, show as fluid sealant surface and substantially black.This is due to fungus growth and to spread, Caused silicone rubber inner molecular structure to destroy biodegradation, its result not only outward appearance by the erosion of mycete and its secretions Very ugly, and the mechanical property of fluid sealant is affected, until lose using function.So using tool under hygrothermal environment The organosilicon sealant having anti-mold effect seems more and more urgent.It is noted that be not in organosilicon sealant simply Add the medicine that some have mildew-proof function just can make the mildew-resistant organosilicon sealant with superior fungicidal properties it is necessary to When consider the various impacts on organosilicon sealant for the anti-fungus material used, comprising: 1. processing performance impact；2. mechanical property shadow Ring；3. adhesive property impact；4. impact of storge quality etc..

Content of the invention

Present invention mainly solves technical problem: for after the silicone sealant adhesive curing of current tradition under hygrothermal environment easily Mould growth, leads to fluid sealant inner molecular structure and destroys, mechanical property reduces and not ageing-resistant defect, and the present invention takes Fresh Egg is soaked in liquor zinci chloridi, boils, and makes zinc ion and protein chelates, regathers albumen mill-drying, Deca alkali Liquid simultaneously adds alkaline protease, makes protein chelates zinc be hydrolyzed into polypeptide chelate zinc, then with ammonia as precipitant, makes polypeptide chelate Zinc element slowly discharges and precipitates calcines to obtain flocculence nano zine oxide, as aging resistance and mouldy composition, then is aided with Folium cinnamomi camphorae Further up to long-acting mould-proof effect, last and the vacuum kneading such as silicone rubber, methyl-silicone oil, filling and sealing obtain final product resistance to old extract Change mould-proof-type organosilicon sealant, the present invention is by zinc element and proteoclastic peptide material complexation, gained after precipitation Nano zine oxide, compensate for traditional organosilicon sealant and there is the not good defect of ageing resistace, then will extract in Folium cinnamomi camphorae Impregnating fluid is consolidated to the antiseptic property of fluid sealant, has broad application prospects.

In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:

(1) collect 10～15 Fresh Eggs, be placed in and fill the plastic tub that 2～4l mass fraction is 8～10% liquor zinci chloridis In, soak 10～15 days, subsequently put into egg in boiling water, cook 10～15min, naturally cool to after room temperature after it, through people Work is separated off eggshell and egg yolk, collects albumen, and albumen is proceeded in colloid mill, grinds 10～15min, after subsequently grinding Albumen particle proceed in baking oven, under the conditions of 80～90 DEG C be dried 8～10h, obtain egg albumen powder；

(2) collect the albumen particle after grinding, proceeded in the beaker filling 400～600ml deionized water, add 2～ 4g alkaline protease, Deca mass fraction is 3～5% sodium hydroxide solutions, adjusts ph to 7.8～8.0, then by beaker amount brought forward Show and test the speed in constant temperature blender with magnetic force, be 60～65 DEG C in temperature, under the conditions of rotating speed is 380～460r/min, constant temperature stirring is anti- Answer 6～8h, adding 60～80ml mass fraction is 10～15% ammonia, stirring reaction 10～15min, then raise temperature to 90～ 95 DEG C, destroy the enzyme treatment 8～10min, centrifugation, abandoning supernatant, collect lower sediment thing；

(3) above-mentioned gained lower sediment thing is proceeded in baking oven, be dried to constant weight under the conditions of 105～110 DEG C, then after being dried Precipitate proceed to Muffle furnace, in temperature be 400～420 DEG C under the conditions of calcination processing 3～5h, cool to room temperature with the furnace, obtain final product Flocculence nano zine oxide, standby；

(4) weigh fresh Folium cinnamomi camphorae 180～200g, be placed in baking oven, be dried to constant weight under the conditions of temperature is 105～110 DEG C, Again dried Folium cinnamomi camphorae is pulverized, cross 40～80 mesh sieves, obtain Folium cinnamomi camphorae powder, then be poured into that to fill 300～400ml anhydrous In the flask of ethanol, it is placed in Microwave Extraction Apparatus, 60～90s is extracted with 400～600w power, filter, remove filtering residue, by filtrate It is placed in beaker, stratification, is separated off water layer, add 15～20g anhydrous sodium sulfate, stand 8～12h, then will be organic Layer proceeds to Rotary Evaporators, concentrated by rotary evaporation 30～45min under the conditions of temperature is 65～70 DEG C, obtains Lignum cinnamomi camphorae leaf extract；

(5) count by weight, take 80～120 part of 107 silicone rubber, 20～40 part of 201 methyl-silicone oil, 8～12 parts of steps successively (3) standby flocculence nano zine oxide, 6～8 parts of methyl tributanoximo silanes, 0.8～1.2 part of silane coupler kh-550, 0.08～0.12 part of dibutyl tin laurate, 1～3 part of above-mentioned gained Lignum cinnamomi camphorae leaf extract, put into planetary kneader, vacuum Stirring kneading 45～60min, filling and sealing, obtain final product ageing-resistant mould-proof-type organosilicon sealant.

The application process of the present invention is: first aluminium alloy and glass being treated, seam crossing acetone is cleared up 2～3 times, is smeared with cleaning Cloth is cleaned, then takes the ageing-resistant mould-proof-type organosilicon sealant that the present invention is obtained, and is coated uniformly on alloy and glass seam Place, control coating thickness is 2～5mm, and after testing, the surface drying time of fluid sealant is 0.5～2.0h, and mould proof grade is up to the superlative degree 0 grade, mouldy, yellowing phenomenon does not occur during use, service life increases by 3～7 years compared with conventional seals glue.

The invention has the beneficial effects as follows:

(1) mildew-resistant organosilicon sealant preparation of the present invention is simple, and anti-mold effect is excellent, low toxicity, the manufacturability of fluid sealant Energy, shelf characteric are excellent；

(2) gained organosilicon sealant ageing-resistant performance of the present invention is excellent, increases by 60～80% compared with conventional seals glue utilization rate, tool There are wide economic outlook, suitable large-scale production and application.

Specific embodiment

Collect 10～15 Fresh Eggs first, being placed in and filling 2～4l mass fraction is moulding of 8～10% liquor zinci chloridis In feed basin, soak 10～15 days, subsequently put into egg in boiling water, cook 10～15min, naturally cool to after room temperature after it, Through being manually separated off eggshell and egg yolk, collect albumen, and albumen is proceeded in colloid mill, grind 10～15min, subsequently will grind Albumen particle after mill proceeds in baking oven, 8～10h is dried, obtains egg albumen powder under the conditions of 80～90 DEG C；Collect the albumen after grinding Particle, is proceeded in the beaker filling 400～600ml deionized water, adds 2～4g alkaline protease, and Deca quality is divided Number is 3～5% sodium hydroxide solutions, adjusts ph to 7.8～8.0, then beaker is proceeded to digital display and test the speed in constant temperature blender with magnetic force, It is 60～65 DEG C in temperature, under the conditions of rotating speed is 380～460r/min, constant temperature stirring reaction 6～8h, add 60～80ml matter Amount fraction is 10～15% ammonia, and stirring reaction 10～15min then raises temperature to 90～95 DEG C, destroy the enzyme treatment 8～10min, from The heart separates, abandoning supernatant, collects lower sediment thing；Above-mentioned gained lower sediment thing is proceeded in baking oven, in 105～110 DEG C Under the conditions of be dried to constant weight, more dried precipitate is proceeded to Muffle furnace, at calcining under the conditions of temperature is 400～420 DEG C Reason 3～5h, cools to room temperature with the furnace, obtains final product flocculence nano zine oxide, standby；Weigh fresh Folium cinnamomi camphorae 180～200g, be placed in In baking oven, it is dried to constant weight under the conditions of temperature is 105～110 DEG C, more dried Folium cinnamomi camphorae is pulverized, cross 40～80 mesh Sieve, obtains Folium cinnamomi camphorae powder, then is poured in the flask filling 300～400ml dehydrated alcohol, be placed in Microwave Extraction Apparatus, with 400～600w power extracts 60～90s, filters, and removes filtering residue, filtrate is placed in beaker, stratification, is separated off water Layer, adds 15～20g anhydrous sodium sulfate, stands 8～12h, then organic layer is proceeded to Rotary Evaporators, is 65～70 in temperature Concentrated by rotary evaporation 30～45min under the conditions of DEG C, obtains Lignum cinnamomi camphorae leaf extract；Count by weight, take 80～120 part of 107 silicon rubber successively Glue, 20～40 part of 201 methyl-silicone oil, 8～12 parts of standby flocculence nano zine oxides, 6～8 parts of methyl tributanoximo silanes, 0.8～1.2 part of silane coupler kh-550,0.08～0.12 part of dibutyl tin laurate, 1～3 part of above-mentioned gained Folium cinnamomi camphorae Extracting solution, puts into planetary kneader, and vacuum stirring mediates 45～60min, filling and sealing, obtains final product ageing-resistant mould-proof-type organosilicon Fluid sealant.

Example 1

Collect 10 Fresh Eggs first, be placed in and fill in the plastic tub that 2l mass fraction is 8% liquor zinci chloridi, soak 10 days, Subsequently egg is put in boiling water, cook 10min, naturally cool to after room temperature after it, through being manually separated off eggshell and egg yolk, Collect albumen, and albumen is proceeded in colloid mill, grind 10min, subsequently proceed to the albumen particle after grinding in baking oven, in 80 8h is dried under the conditions of DEG C, obtains egg albumen powder；Collect the albumen particle after grinding, proceeded to the beaker filling 400ml deionized water In, add 2g alkaline protease, Deca mass fraction is 3% sodium hydroxide solution, adjusts ph to 7.8, then by beaker amount brought forward Show and test the speed in constant temperature blender with magnetic force, be 60 DEG C in temperature, under the conditions of rotating speed is 380r/min, constant temperature stirring reaction 6h, then plus Entering 60ml mass fraction is 10% ammonia, and stirring reaction 10min then raises temperature to 90 DEG C, destroy the enzyme treatment 8min, and centrifugation is abandoned Remove supernatant, collect lower sediment thing；Above-mentioned gained lower sediment thing is proceeded in baking oven, is dried to perseverance under the conditions of 105 DEG C Weight, more dried precipitate is proceeded to Muffle furnace, calcination processing 3h under the conditions of temperature is 400 DEG C, cool to room temperature with the furnace, Obtain final product flocculence nano zine oxide, standby；Weigh fresh Folium cinnamomi camphorae 180g, be placed in baking oven, dry under the conditions of temperature is 105 DEG C Dry more dried Folium cinnamomi camphorae is pulverized to constant weight, cross 40 mesh sieves, obtain Folium cinnamomi camphorae powder, then be poured into that to fill 300ml anhydrous In the flask of ethanol, it is placed in Microwave Extraction Apparatus, 60s is extracted with 400w power, filter, remove filtering residue, filtrate is placed in beaker In, stratification, it is separated off water layer, adds 15g anhydrous sodium sulfate, stand 8h, then organic layer is proceeded to Rotary Evaporators, Concentrated by rotary evaporation 30min under the conditions of temperature is 65 DEG C, obtains Lignum cinnamomi camphorae leaf extract；Count by weight, take 80 part of 107 silicon rubber successively Glue, 20 part of 201 methyl-silicone oil, 8 parts of standby flocculence nano zine oxides, 6 parts of methyl tributanoximo silanes, 0.8 part of silane is even Connection agent kh-550,0.08 part of dibutyl tin laurate, 1 part of above-mentioned gained Lignum cinnamomi camphorae leaf extract, put into planetary kneader, very 45min, filling and sealing are mediated in empty stirring, obtain final product ageing-resistant mould-proof-type organosilicon sealant.

The application process of the present invention is: first will be cleared up 2 times with acetone at aluminium alloy and glass mouth to be sealed, uses clean rag Clean, then take the ageing-resistant mould-proof-type organosilicon sealant that the present invention is obtained, be coated uniformly on alloy and glass seam crossing, Control coating thickness is 2mm, and after testing, the surface drying time of fluid sealant is 0.5h, mould proof grade up to highest 0 grade, using Mouldy, yellowing phenomenon does not occur in journey, service life increases by 3 years compared with conventional seals glue.

Example 2

Collect 15 Fresh Eggs first, be placed in and fill in the plastic tub that 4l mass fraction is 10% liquor zinci chloridi, soak 15 My god, subsequently egg is put in boiling water, cook 15min, naturally cool to after room temperature after it, through being manually separated off eggshell and egg Huang, collects albumen, and albumen is proceeded in colloid mill, grinds 15min, subsequently proceeds in baking oven by the albumen particle after grinding, 10h is dried under the conditions of 90 DEG C, obtains egg albumen powder；Collect the albumen particle after grinding, proceeded to and fill 600ml deionized water In beaker, add 4g alkaline protease, Deca mass fraction is 5% sodium hydroxide solution, adjusts ph to 8.0, then beaker is turned Enter digital display to test the speed in constant temperature blender with magnetic force, be 65 DEG C in temperature, under the conditions of rotating speed is 460r/min, constant temperature stirring reaction 8h, Adding 80ml mass fraction is 15% ammonia, and stirring reaction 15min then raises temperature to 95 DEG C, destroy the enzyme treatment 10min, centrifugation point From, abandoning supernatant, collect lower sediment thing；Above-mentioned gained lower sediment thing is proceeded in baking oven, is dried under the conditions of 110 DEG C To constant weight, more dried precipitate is proceeded to Muffle furnace, calcination processing 5h under the conditions of temperature is 420 DEG C, cool to the furnace Room temperature, obtains final product flocculence nano zine oxide, standby；Weigh fresh Folium cinnamomi camphorae 200g, be placed in baking oven, be 110 DEG C of bars in temperature It is dried to constant weight under part, more dried Folium cinnamomi camphorae is pulverized, cross 80 mesh sieves, obtain Folium cinnamomi camphorae powder, then be poured into and fill In the flask of 400ml dehydrated alcohol, it is placed in Microwave Extraction Apparatus, 90s is extracted with 600w power, filter, remove filtering residue, by filtrate It is placed in beaker, stratification, is separated off water layer, add 20g anhydrous sodium sulfate, stand 12h, then organic layer is proceeded to rotation Turn evaporimeter, concentrated by rotary evaporation 45min under the conditions of temperature is 70 DEG C, obtain Lignum cinnamomi camphorae leaf extract；Count by weight, take successively 120 part of 107 silicone rubber, 40 part of 201 methyl-silicone oil, 12 parts of standby flocculence nano zine oxides, 8 parts of methyl tributanoximo silicon Alkane, 1.2 parts of silane coupler kh-550,0.12 part of dibutyl tin laurate, 3 parts of above-mentioned gained Lignum cinnamomi camphorae leaf extracts, put into Planetary kneader, vacuum stirring mediates 60min, filling and sealing, obtains final product ageing-resistant mould-proof-type organosilicon sealant.

The application process of the present invention is: first will be cleared up 3 times with acetone at aluminium alloy and glass mouth to be sealed, uses clean rag Clean, then take the ageing-resistant mould-proof-type organosilicon sealant that the present invention is obtained, be coated uniformly on alloy and glass seam crossing, Control coating thickness is 5mm, and after testing, the surface drying time of fluid sealant is 2.0h, mould proof grade up to highest 0 grade, using Mouldy, yellowing phenomenon does not occur in journey, service life increases by 7 years compared with conventional seals glue.

Example 3

Collect 13 Fresh Eggs first, be placed in and fill in the plastic tub that 3l mass fraction is 9% liquor zinci chloridi, soak 13 days, Subsequently egg is put in boiling water, cook 13min, naturally cool to after room temperature after it, through being manually separated off eggshell and egg yolk, Collect albumen, and albumen is proceeded in colloid mill, grind 13min, subsequently proceed to the albumen particle after grinding in baking oven, in 85 9h is dried under the conditions of DEG C, obtains egg albumen powder；Collect the albumen particle after grinding, proceeded to the beaker filling 500ml deionized water In, add 3g alkaline protease, Deca mass fraction is 4% sodium hydroxide solution, adjusts ph to 7.9, then by beaker amount brought forward Show and test the speed in constant temperature blender with magnetic force, be 63 DEG C in temperature, under the conditions of rotating speed is 420r/min, constant temperature stirring reaction 7h, then plus Entering 70ml mass fraction is 13% ammonia, and stirring reaction 13min then raises temperature to 93 DEG C, destroy the enzyme treatment 9min, and centrifugation is abandoned Remove supernatant, collect lower sediment thing；Above-mentioned gained lower sediment thing is proceeded in baking oven, is dried to perseverance under the conditions of 107 DEG C Weight, more dried precipitate is proceeded to Muffle furnace, calcination processing 4h under the conditions of temperature is 410 DEG C, cool to room temperature with the furnace, Obtain final product flocculence nano zine oxide, standby；Weigh fresh Folium cinnamomi camphorae 190g, be placed in baking oven, dry under the conditions of temperature is 107 DEG C Dry more dried Folium cinnamomi camphorae is pulverized to constant weight, cross 60 mesh sieves, obtain Folium cinnamomi camphorae powder, then be poured into that to fill 350ml anhydrous In the flask of ethanol, it is placed in Microwave Extraction Apparatus, 80s is extracted with 500w power, filter, remove filtering residue, filtrate is placed in beaker In, stratification, it is separated off water layer, adds 17g anhydrous sodium sulfate, stand 10h, then organic layer is proceeded to rotary evaporation Instrument, concentrated by rotary evaporation 38min under the conditions of temperature is 67 DEG C, obtain Lignum cinnamomi camphorae leaf extract；Count by weight, take 100 part 107 successively Silicone rubber, 30 part of 201 methyl-silicone oil, 10 parts of standby flocculence nano zine oxides, 7 parts of methyl tributanoximo silanes, 1.0 parts of silicon Alkane coupling agent kh-550,1.10 parts of dibutyl tin laurates, 2 parts of above-mentioned gained Lignum cinnamomi camphorae leaf extracts, put into planetary kneading Machine, vacuum stirring mediates 52min, filling and sealing, obtains final product ageing-resistant mould-proof-type organosilicon sealant.

The application process of the present invention is: first will be cleared up 2.5 times with acetone at aluminium alloy and glass mouth to be sealed, is smeared with cleaning Cloth is cleaned, then takes the ageing-resistant mould-proof-type organosilicon sealant that the present invention is obtained, and is coated uniformly on alloy and glass seam Place, control coating thickness is 4mm, and after testing, the surface drying time of fluid sealant is 1.3h, and mould proof grade, up to highest 0 grade, uses During mouldy, yellowing phenomenon does not occur, service life compared with conventional seals glue increase by 5 years.

Claims (1)

1. a kind of preparation method of ageing-resistant mould-proof-type organosilicon sealant is it is characterised in that concrete preparation process is:

(1) collect 10～15 Fresh Eggs, be placed in and fill the plastic tub that 2～4l mass fraction is 8～10% liquor zinci chloridis In, soak 10～15 days, subsequently put into egg in boiling water, cook 10～15min, naturally cool to after room temperature after it, through people Work is separated off eggshell and egg yolk, collects albumen, and albumen is proceeded in colloid mill, grinds 10～15min, after subsequently grinding Albumen particle proceed in baking oven, under the conditions of 80～90 DEG C be dried 8～10h, obtain egg albumen powder；

(2) collect the albumen particle after grinding, proceeded in the beaker filling 400～600ml deionized water, add 2～ 4g alkaline protease, Deca mass fraction is 3～5% sodium hydroxide solutions, adjusts ph to 7.8～8.0, then by beaker amount brought forward Show and test the speed in constant temperature blender with magnetic force, be 60～65 DEG C in temperature, under the conditions of rotating speed is 380～460r/min, constant temperature stirring is anti- Answer 6～8h, adding 60～80ml mass fraction is 10～15% ammonia, stirring reaction 10～15min, then raise temperature to 90～ 95 DEG C, destroy the enzyme treatment 8～10min, centrifugation, abandoning supernatant, collect lower sediment thing；

(3) above-mentioned gained lower sediment thing is proceeded in baking oven, be dried to constant weight under the conditions of 105～110 DEG C, then after being dried Precipitate proceed to Muffle furnace, in temperature be 400～420 DEG C under the conditions of calcination processing 3～5h, cool to room temperature with the furnace, obtain final product Flocculence nano zine oxide, standby；

(4) weigh fresh Folium cinnamomi camphorae 180～200g, be placed in baking oven, be dried to constant weight under the conditions of temperature is 105～110 DEG C, Again dried Folium cinnamomi camphorae is pulverized, cross 40～80 mesh sieves, obtain Folium cinnamomi camphorae powder, then be poured into that to fill 300～400ml anhydrous In the flask of ethanol, it is placed in Microwave Extraction Apparatus, 60～90s is extracted with 400～600w power, filter, remove filtering residue, by filtrate It is placed in beaker, stratification, is separated off water layer, add 15～20g anhydrous sodium sulfate, stand 8～12h, then will be organic Layer proceeds to Rotary Evaporators, concentrated by rotary evaporation 30～45min under the conditions of temperature is 65～70 DEG C, obtains Lignum cinnamomi camphorae leaf extract；

(5) count by weight, take 80～120 part of 107 silicone rubber, 20～40 part of 201 methyl-silicone oil, 8～12 parts of steps successively (3) standby flocculence nano zine oxide, 6～8 parts of methyl tributanoximo silanes, 0.8～1.2 part of silane coupler kh-550, 0.08～0.12 part of dibutyl tin laurate, 1～3 part of above-mentioned gained Lignum cinnamomi camphorae leaf extract, put into planetary kneader, vacuum Stirring kneading 45～60min, filling and sealing, obtain final product ageing-resistant mould-proof-type organosilicon sealant.